CN116351394A - Method for preparing porous adsorption material by utilizing gasified fine ash - Google Patents

Method for preparing porous adsorption material by utilizing gasified fine ash Download PDF

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CN116351394A
CN116351394A CN202310233743.2A CN202310233743A CN116351394A CN 116351394 A CN116351394 A CN 116351394A CN 202310233743 A CN202310233743 A CN 202310233743A CN 116351394 A CN116351394 A CN 116351394A
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acid
acid treatment
fine ash
treatment
metal salt
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何国锋
柳金秋
孙海勇
李磊
段静
刘烨炜
严健
常秋连
王成江
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Ccteg Clean Energy Co ltd
Middling Coal Shaanxi Energy And Chemical Group Co ltd
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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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    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01J20/0237—Compounds of Cu
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    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
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    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes

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Abstract

The invention relates to a method for preparing a porous adsorption material by utilizing gasified fine ash, which comprises the following steps: (1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying; (2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment, cooling, and performing acid washing, washing and drying to obtain the porous adsorption material. The method provided by the invention realizes the preparation of the adsorption material with high specific surface area by the specific design of the preparation process and the cooperation of specific acid treatment, subsequent alkali, metal salt and thermal activation treatment, and the specific surface area of the obtained adsorption material is more than or equal to 1546.23m 2 /g。

Description

Method for preparing porous adsorption material by utilizing gasified fine ash
Technical Field
The invention relates to the technical field of solid waste resource utilization, in particular to a method for preparing a porous adsorption material by utilizing gasified fine ash.
Background
At present, the entrained flow coal gasification technology has the advantages of wide coal adaptability, high gasification temperature, high gasification efficiency, large production capacity, environmental friendliness and the like, and becomes the most widely used technology in the coal gasification industry in China at present. However, a great amount of ash generated by entrained flow gasification occupies a great amount of land and causes a certain pollution to the soil only by accumulation landfill treatment, and particularly, the gasification fine ash contains higher residual carbon, and the recycling utilization of the ash becomes a difficult problem to be solved.
The prior art mainly adopts the way of recycling gasified fine ash by blending combustion, preparing building materials, preparing adsorption materials, serving as soil amendment, preparing adsorption materials, catalysts and the like.
CN115672334a discloses that the active component nickel is introduced and modified by adopting different auxiliary agents by taking gasified ash as a carrier, so that the problem that a single active component is easy to deactivate in the catalytic process is solved, and the potential of realizing the full-component utilization of gasified products is provided.
CN115571890a discloses a method for preparing polymeric aluminum ferric silicate flocculant by gasified slag and application thereof, the turbidity removal rate of steel wastewater reaches 93.7%, the chromaticity removal rate reaches 36.5%, the COD removal rate reaches 71.0%, and the method has good effect of reducing turbidity, chromaticity and COD of the wastewater.
CN115634562a discloses CaO, mgO, na in utilizing gangue, fly ash, gasified ash and desulfurized gypsum 2 O、K 2 O、Fe 2 O 3 Etc. as active ingredient with CO 2 Reaction to realize CO 2 Is absorbed and solidified by CO 2 The absorption capacity of the material can reach more than 0.30g/g of the material.
CN114849646a discloses a modified gasified slag active carbon adsorption material, and the collected gasified slag and binder (coal tar, pitch) are kneaded, and the modified gasified slag active carbon adsorption material is finally obtained through the processes of granulation, pyrolysis carbonization, oxidation, drying, reduction, calcination and the like.
In summary, the disclosed gasification ash recycling method shows that the gasification ash has higher adsorption and utilization value potential, but the problems that the pore distribution and the comparison area of the gasification fine ash generated by different gasification processes are greatly different, the pore characteristic parameters of the fine ash and the active carbon have large gaps and the like are solved, the adsorption and utilization values of the gasification fine ash are adversely affected, and further, the existing treatment method cannot fully develop the adsorption values of the gasification fine ash due to higher carbon and ash contents in the gasification fine ash.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for preparing a porous adsorption material by utilizing gasified fine ash, so as to solve the problems of high ash content and lower adsorption performance of the gasified fine ash based adsorption material in the prior art.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing a porous adsorption material by utilizing gasified fine ash, which comprises the following steps:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment, cooling, and performing acid washing, washing and drying to obtain the porous adsorption material.
The method provided by the invention realizes the preparation of the adsorption material with high specific surface area by the specific design of the preparation process and the cooperation of specific acid treatment, subsequent alkali, metal salt and heat activation treatment.
In the present invention, the gasified fine ash mainly includes unburned carbon and ash.
In the invention, the washing after the acid treatment is water washing or alcohol washing and the like until the pH value of the washing water is 6-7.
In the present invention, the heat activation treatment is performed under a protective atmosphere, which may be 1 or a combination of at least 2 of carbon dioxide, nitrogen, an inert gas such as helium, neon, argon, and the like.
In the invention, acid liquor (such as hydrochloric acid, nitric acid or sulfuric acid with the mass concentration of 20-80 percent) is adopted after the heat activation treatment, and concentrated hydrochloric acid is adopted when the concentration is overlarge, and other acids are analogized in sequence) for pickling for 5-60 minutes.
In the present invention, the washing after the heat activation treatment is performed by washing with water or alcohol until the pH of the washing water is 6 to 7.
In a preferred embodiment of the present invention, the dry ash content of the gasified fine ash in the step (1) is 40 to 70% by mass, and may be, for example, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%, etc., but not limited to the recited values, and other non-recited values in the range are equally applicable.
Preferably, the water content of the gasified fine ash in the step (1) is 60-70% by mass, for example, 60%, 60.5%, 61%, 61.5%, 62%, 62.5%, 63%, 63.5%, 64%, 64.5%, 65%, 65.5%, 66%, 66.5%, 67%, 67.5%, 68%, 68.5%, 69%, 69.5% or 70%, etc., but not limited to the recited values, and other non-recited values in the range are equally applicable.
As a preferred technical scheme of the invention, the mass ratio of the acid and the gasified fine ash dry basis used in the acid treatment in the step (1) is 1 (1-1.2), for example, 1:1, 1:1.01, 1:1.02, 1:1.03, 1:1.04, 1:1.05, 1:1.06, 1:1.07, 1:1.08, 1:1.09, 1:1.1, 1:1.11, 1:1.12, 1:1.13, 1:1.14, 1:1.15, 1:1.16, 1:1.17, 1:1.18, 1:1.19 or 1:1.2 can be exemplified, but the invention is not limited to the exemplified values, and other non-exemplified values in the range are equally applicable.
As a preferred embodiment of the present invention, the acid used in the acid treatment in the step (1) comprises 1 or a combination of at least 2 of concentrated hydrochloric acid, concentrated nitric acid or concentrated sulfuric acid.
In a preferred embodiment of the present invention, the temperature of the acid treatment in the step (1) is 50 to 90℃and may be, for example, 50℃52℃54℃56℃58℃60℃62℃64℃66℃68℃70℃72℃74℃76℃78℃80℃82℃84℃86℃88℃90℃or 90℃but not limited to the values listed and other values not listed in this range are equally applicable.
Preferably, the acid treatment in step (1) is performed for a period of time ranging from 2 to 2.5 hours, such as 2 hours, 2.02 hours, 2.04 hours, 2.06 hours, 2.08 hours, 2.1 hours, 2.12 hours, 2.14 hours, 2.16 hours, 2.18 hours, 2.2 hours, 2.22 hours, 2.24 hours, 2.26 hours, 2.28 hours, 2.3 hours, 2.32 hours, 23.4 hours, 2.36 hours, 2.38 hours, 2.4 hours, 2.42 hours, 2.44 hours, 2.46 hours, 2.48 hours, or 2.5 hours, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
In a preferred embodiment of the present invention, the water content of the acid-treated material in the step (1) is 3% by mass or less, and may be, for example, 3%, 2.9%, 2.8%, 2.7%, 2.6%, 2.5%, 2.4%, 2.3%, 2.2%, 2.1%, 2%, 1.9%, 1.8%, 1.7%, 1.6%, 1.5%, 1.4%, 1.3%, 1.2%, 1.1% or 1%, etc., but the water content is not limited to the above-mentioned values, and other non-mentioned values are equally applicable in the above range.
Preferably, the particle size of the acid treatment material in the mixing in the step (2) is less than or equal to 0.5mm.
In the present invention, the particle size of the acid-treated material in the mixing may be an aggregate of particles of a single particle size within a defined range, or an aggregate of all particles within a certain particle size range, such as an aggregate of particles having a particle size of 0.1mm, such as an aggregate of particles having a particle size of 0.01mm, such as an aggregate of all particles within a particle size range of 0.2 to 0.4mm, such as an aggregate of all particles within a particle size range of 0.1 to 0.3mm, such as an aggregate of all particles within a particle size range of 0.01 to 0.4mm, or the like.
As a preferred embodiment of the present invention, the alkali in step (2) comprises 1 or a combination of at least 2 of sodium hydroxide, potassium hydroxide or calcium hydroxide.
Preferably, the metal salt of step (2) comprises a copper salt and/or a nickel salt.
In the present invention, the copper salt may be copper sulfate, copper chloride, copper nitrate, basic copper carbonate, or the like.
In the present invention, the nickel salt may be nickel sulfate, nickel chloride, nickel nitrate, basic nickel carbonate, or the like.
As a preferred embodiment of the present invention, the mass ratio of the alkali and the metal salt in the step (2) is 1 (0.05-0.2), for example, 1:0.05, 1:0.055, 1:0.06, 1:0.065, 1:0.07, 1:0.075, 1:0.08, 1:0.085, 1:0.09, 1:0.095, 1:0.1, 1:0.105, 1:0.11, 1:0.115, 1:0.12, 1:0.125, 1:0.13, 1:0.135, 1:0.14, 1:0.145, 1:0.15, 1:0.155, 1:0.16, 1:0.165, 1:0.17, 1:0.175, 1:0.18, 1:0.185, 1:0.19, 1:0.195, or 1:0.2, etc., but the present invention is not limited to the same numerical values as those enumerated above.
Preferably, the mass ratio of the gasified fine ash dry basis to the mixture of alkali and metal salt in the mixing in step (2) is 1 (3-4), and may be, for example, 1:3, 1:3.02, 1:3.04, 1:3.06, 1:3.08, 1:3.1, 1:3.12, 1:3.14, 1:3.16, 1:3.18, 1:3.2, 1:3.22, 1:3.24, 1:3.26, 1:3.28, 1:3.3, 1:3.32, 1:3.34, 1:3.36, 1:3.38, 1:3.4, 1:3.42, 1:3.44, 1:3.46, 1:3.48, 1:3.5, 1:3.52, 1:3.54, 1:3.56, 1:3.58, 1:3.6, 1:3.62, 1:3.64, 1:3.66, 1:3.68, 1:3.58, 1:3.6, 1:3.82, 1:3.6, 1:3.74, 1:3.9, 1:3.82, 1:3.46, 1:3.9, 1:3.6, 1:3.9, 1:3.82, 1:3.9, 1:3.8, 1:3.9, 1:3.82, 1:3.9, 1, 1:3.9, and the like, which are not limited to the above.
In a preferred embodiment of the present invention, the temperature of the heat-activation treatment in the step (2) is 850 to 900 ℃, for example, 850 ℃, 852 ℃, 854 ℃, 856 ℃, 858 ℃, 860 ℃, 862 ℃, 864 ℃, 866 ℃, 870 ℃, 872 ℃, 874 ℃, 876 ℃, 878 ℃, 880 ℃, 882 ℃, 884 ℃, 886 ℃, 888 ℃, 890 ℃, 892 ℃, 894 ℃, 896 ℃, 898 ℃, or 900 ℃, etc., but the heat-activation treatment is not limited to the above-mentioned values, and other values not mentioned in the above range are equally applicable.
Preferably, the time of the heat activation treatment in step (2) is 1-2h, and may be, for example, 1h, 1.02h, 1.04h, 1.06h, 1.08h, 1.1h, 1.12h, 1.14h, 1.16h, 1.18h, 1.2h, 1.22h, 1.24h, 1.26h, 1.28h, 1.3h, 1.32h, 1.34h, 1.36h, 1.38h, 1.4h, 1.42h, 1.44h, 1.46h, 1.48h, 1.5h, 1.52h, 1.54h, 1.56h, 1.58h, 1.6h, 1.62h, 1.64h, 1.66h, 1.68h, 1.7h, 1.72h, 1.74h, 1.76h, 1.78h, 1.8h, 1.82h, 1.84h, 1.86, 1.92h, 1.88h, 1.98h, or the like, but is not limited to the other suitable ranges.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 40-70% by mass percent; the water content of the gasified fine ash is 60-70% by mass percent; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1 (1-1.2); the acid used in the acid treatment comprises 1 or a combination of at least 2 of concentrated hydrochloric acid, concentrated nitric acid or concentrated sulfuric acid; the temperature of the acid treatment is 50-90 ℃; the acid treatment time is 2-2.5h; the water content of the acid treatment material is less than or equal to 3 percent by mass percent;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment, cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the base of step (2) comprises 1 or a combination of at least 2 of sodium hydroxide, potassium hydroxide or calcium hydroxide; the metal salt comprises copper salt and/or nickel salt; the mass ratio of the alkali to the metal salt is 1 (0.05-0.2); the particle size of the acid treatment material in the mixing is less than or equal to 0.5mm; the mass ratio of the gasification fine ash dry basis to the mixture composed of alkali and metal salt in the mixing is 1 (3-4); the temperature of the heat activation treatment is 850-900 ℃; the time of the heat activation treatment is 1-2h.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, gasified fine ash and acid are mixed, heated and pre-reacted, so that the efficiency of thermal activation treatment is improved, the influence of unstable ash on the reaming effect in the thermal activation treatment process is reduced, the porosity of the fine ash is improved, the specific surface area of the fine ash is increased, the fine ash reacts with stable ash to generate active ash with relatively high reactivity through the multi-point activation of alkali and metal salt under the high-temperature condition, and the adsorption action active point is increased. After heat activation treatment, the ash with more reactive reactivity reacts with acid to achieve the effects of further ash reduction and hole expansion, thereby obtaining the gasified fine ash-based adsorption material with extremely low ash content and higher specific surface area, and the specific surface area of the obtained adsorption material is more than or equal to 1546.23m 2 /g。
Drawings
Fig. 1 is a flowchart of a method for preparing a porous adsorption material by gasifying fine ash according to an embodiment of the present invention.
The present invention will be described in further detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
Detailed Description
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
as can be seen from fig. 1, the gasified fine ash is subjected to acid treatment, acid washing, washing and drying to obtain an acid treated material, then the acid treated material is mixed with alkali and metal salt, and then heat activation treatment is performed, and after the heat activation treatment, the gasified fine ash based porous adsorption material is obtained through washing and drying.
Specific examples are as follows:
example 1
The present embodiment provides a method for preparing a porous adsorption material using gasified fine ash, the method comprising the steps of:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 48.13 percent by mass percent; the water content of the gasified fine ash is 66.5 percent by mass; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1:1.1; the acid used in the acid treatment is concentrated hydrochloric acid; the temperature of the acid treatment is 50 ℃; the acid treatment time is 2 hours; the water content of the acid treatment material is 3 percent by mass percent;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment (carbon dioxide atmosphere), cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the alkali in the step (2) is sodium hydroxide; the metal salt is copper chloride; the mass ratio of the alkali to the metal salt is 1:0.15; the acid treatment material in the mixing is an aggregate with the particle size less than or equal to 0.5mm; the mass ratio of the gasification fine ash dry basis to the mixture consisting of alkali and metal salt in the mixing is 1:3; the temperature of the heat activation treatment is 900 ℃; the time of the heat activation treatment is 2 hours; the pickling is carried out by adopting hydrochloric acid with the mass concentration of 20 percent for 50 minutes.
The performance index of the obtained porous adsorption material is shown in Table 1.
Example 2
The present embodiment provides a method for preparing a porous adsorption material using gasified fine ash, the method comprising the steps of:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 62.04 percent by mass percent; the water content of the gasified fine ash is 68.4 percent by mass; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1:1.2; the acid used in the acid treatment is concentrated sulfuric acid; the temperature of the acid treatment is 90 ℃; the acid treatment time is 2.5h; the water content of the acid treatment material is 2% by mass percent;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment (carbon dioxide atmosphere), cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the alkali in the step (2) is potassium hydroxide; the metal salt is copper chloride; the mass ratio of the alkali to the metal salt is 1:0.2; the acid treatment material in the mixing is an aggregate with the particle size less than or equal to 0.1 mm; the mass ratio of the gasification fine ash dry basis to the mixture consisting of alkali and metal salt in the mixing is 1:3.5; the temperature of the heat activation treatment is 900 ℃; the time of the heat activation treatment is 2 hours; the pickling is carried out by adopting sulfuric acid with the mass concentration of 80 percent for 5min.
The performance index of the obtained porous adsorption material is shown in Table 1.
Example 3
The present embodiment provides a method for preparing a porous adsorption material using gasified fine ash, the method comprising the steps of:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 66.48 percent by mass percent; the water content of the gasified fine ash is 65.14 percent by mass; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1:1; the acid used in the acid treatment is concentrated sulfuric acid; the temperature of the acid treatment is 80 ℃; the acid treatment time is 2 hours; the water content of the acid treatment material is 3 percent by mass percent;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment (argon), cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the alkali in the step (2) is potassium hydroxide; the metal salt comprises copper salt and/or nickel salt; the mass ratio of the alkali to the metal salt is 1:0.05; aggregate with particle size less than or equal to 0.075mm of acid treatment material in the mixing; the mass ratio of the gasification fine ash dry basis to the mixture consisting of alkali and metal salt in the mixing is 1:4; the temperature of the heat activation treatment is 850 ℃; the time of the heat activation treatment is 1h; the pickling is carried out by adopting nitric acid with the mass concentration of 40% for 30min.
The performance index of the obtained porous adsorption material is shown in Table 1.
Example 4
The present embodiment provides a method for preparing a porous adsorption material using gasified fine ash, the method comprising the steps of:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 42.82 percent by mass percent; the water content of the gasified fine ash is 64% by mass percent; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1:1; the acid used in the acid treatment is concentrated nitric acid; the temperature of the acid treatment is 70 ℃; the acid treatment time is 2 hours; the water content of the acid treatment material is 1% by mass;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment (nitrogen), cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the alkali calcium hydroxide in the step (2); the metal salt is nickel chloride; the mass ratio of the alkali to the metal salt is 1:0.1; the acid treatment material in the mixing is an aggregate with the particle size less than or equal to 0.2 mm; the mass ratio of the gasification fine ash dry basis to the mixture consisting of alkali and metal salt in the mixing is 1:3; the temperature of the heat activation treatment is 900 ℃; the time of the heat activation treatment is 1h; the pickling is carried out by adopting nitric acid with the mass concentration of 50 percent for 30 minutes.
The performance index of the obtained porous adsorption material is shown in Table 1.
Example 5
The only difference from example 1 is that no acid treatment was performed. The gasified fine ash is directly subjected to the step (2) after being washed and dried. The performance index of the obtained porous adsorption material is shown in Table 1.
Example 6
The only difference from example 1 is that no alkali and metal salts are used during the thermal activation. The performance index of the obtained porous adsorption material is shown in Table 1.
Example 7
The only difference from example 1 is that no metal salts are used during the thermal activation. The performance index of the obtained porous adsorption material is shown in Table 1.
Example 8
The only difference from example 1 is that no acid wash is used after thermal activation. The performance index of the obtained porous adsorption material is shown in Table 1.
TABLE 1
Figure BDA0004121291460000101
Figure BDA0004121291460000111
The porous adsorption materials obtained in examples 1-8 were tested for iodine adsorption performance with specific reference to national standard GB/T7702.7-2008, and the specific results are shown in Table 2 below:
TABLE 2
Iodine adsorption value/mg.g -1
Example 1 1597
Example 2 1876
Example 3 1721
Example 4 2120
Example 5 1089
Example 6 525
Example 7 1402
Example 8 894
It is understood that the adsorption material provided in the present invention has good adsorption performance, and the adsorption example is only an illustrative example, and is not limited to iodine, but may be other substances similar to iodine.
It is stated that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e., it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.

Claims (10)

1. A method for preparing a porous adsorption material by using gasified fine ash, which is characterized by comprising the following steps:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment, cooling, and performing acid washing, washing and drying to obtain the porous adsorption material.
2. The method of claim 1, wherein the dry ash content of the gasified fine ash in step (1) is 40-70% by mass;
preferably, the water content of the gasified fine ash in the step (1) is 60-70% by mass.
3. The method according to claim 1 or 2, wherein the mass ratio of the acid used in the acid treatment of step (1) to the gasified fine ash dry basis is 1 (1-1.2).
4. A method according to any one of claims 1 to 3, wherein the acid used in the acid treatment of step (1) comprises 1 or a combination of at least 2 of concentrated hydrochloric acid, concentrated nitric acid or concentrated sulfuric acid.
5. The method of any one of claims 1-4, wherein the temperature of the acid treatment of step (1) is 50-90 ℃;
preferably, the acid treatment in step (1) is carried out for a period of time ranging from 2 to 2.5 hours.
6. The method according to any one of claims 1 to 5, wherein the acid-treated material in step (1) has a water content of 3% or less by mass;
preferably, the particle size of the acid treatment material in the mixing in the step (2) is less than or equal to 0.5mm.
7. The method of any one of claims 1-6, wherein the base of step (2) comprises 1 or a combination of at least 2 of sodium hydroxide, potassium hydroxide, or calcium hydroxide;
preferably, the metal salt of step (2) comprises a copper salt and/or a nickel salt.
8. The method according to any one of claims 1 to 7, wherein the mass ratio of the alkali and the metal salt in step (2) is 1 (0.05 to 0.2);
preferably, the mass ratio of the gasification fine ash dry basis to the mixture composed of alkali and metal salt in the mixing in the step (2) is 1 (3-4).
9. The method of any one of claims 1-8, wherein the temperature of the thermal activation treatment of step (2) is 850-900 ℃;
preferably, the time of the heat activation treatment in the step (2) is 1-2 hours.
10. The method according to any one of claims 1-9, characterized in that the method comprises the steps of:
(1) Acid treatment is carried out on the gasified fine ash, and then the acid treatment material is obtained through cleaning and drying;
the dry ash content of the gasified fine ash in the step (1) is 40-70% by mass percent; the water content of the gasified fine ash is 60-70% by mass percent; the mass ratio of the acid to the gasified fine ash dry basis used in the acid treatment is 1 (1-1.2); the acid used in the acid treatment comprises 1 or a combination of at least 2 of concentrated hydrochloric acid, concentrated nitric acid or concentrated sulfuric acid; the temperature of the acid treatment is 50-90 ℃; the acid treatment time is 2-2.5h; the water content of the acid treatment material is less than or equal to 3 percent by mass percent;
(2) Mixing alkali, metal salt and the acid treatment material obtained in the step (1), performing heat activation treatment, cooling, and performing acid washing, washing and drying to obtain a porous adsorption material;
the base of step (2) comprises 1 or a combination of at least 2 of sodium hydroxide, potassium hydroxide or calcium hydroxide; the metal salt comprises copper salt and/or nickel salt; the mass ratio of the alkali to the metal salt is 1 (0.05-0.2); the particle size of the acid treatment material in the mixing is less than or equal to 0.5mm; the mass ratio of the gasification fine ash dry basis to the mixture composed of alkali and metal salt in the mixing is 1 (3-4); the temperature of the heat activation treatment is 850-900 ℃; the time of the heat activation treatment is 1-2h.
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