CN113522234A - Sulfur dioxide adsorption material and preparation method thereof - Google Patents

Sulfur dioxide adsorption material and preparation method thereof Download PDF

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Publication number
CN113522234A
CN113522234A CN202110719360.7A CN202110719360A CN113522234A CN 113522234 A CN113522234 A CN 113522234A CN 202110719360 A CN202110719360 A CN 202110719360A CN 113522234 A CN113522234 A CN 113522234A
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copper nitrate
activated carbon
sulfur dioxide
mixture
nitrate solution
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CN202110719360.7A
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杨森
杨欢
徐淑权
赵耀辉
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No 59 Research Institute of China Ordnance Industry
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No 59 Research Institute of China Ordnance Industry
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/30Sulfur compounds
    • B01D2257/302Sulfur oxides

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a preparation method of a sulfur dioxide adsorbing material, which comprises the following steps: s100, preparing copper nitrate solution by using copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 0.25-2 mol/L; s200, taking 100 parts of copper nitrate solution obtained in the previous step in proportion, uniformly stirring, and soaking the mixture for 11-15 h at normal temperature; s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 7.5-9 h in an air temperature environment of 88-92 ℃ to complete activation; s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material. And also comprises a sulfur dioxide adsorbing material. The invention provides a sulfur dioxide adsorbing material and a preparation method thereof, which combine activated carbon as a raw material of the adsorbing material and provide the preparation method thereof, and obviously improve the adsorption efficiency and the adsorption capacity of the adsorbing material.

Description

Sulfur dioxide adsorption material and preparation method thereof
Technical Field
The invention relates to the technical field of gas adsorbing materials, in particular to a sulfur dioxide adsorbing material and a preparation method thereof.
Background
The sulfur dioxide is used as an air pollutant and corrosive atmosphere, and the sulfur dioxide is treated by active carbon dry adsorption, so that the method has the advantages of small equipment corrosion, no waste acid and waste water and the like. But the common active carbon has slow desulfurization reaction speed and low adsorption capacity, so the application of the common active carbon is limited to a great extent, and the novel efficient adsorption material can obviously improve the adsorption efficiency and the adsorption capacity. The modified active carbon prepared by the impregnation method at present has high impregnation process conditions and complex impregnation liquid formula.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a method for producing a sulfur dioxide adsorbent.
The technical scheme of the invention is as follows: a preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing copper nitrate solution by using copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 0.25-2 mol/L;
s200, taking 100 parts of copper nitrate solution obtained in the previous step in proportion, adding 50 parts of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 93-96 ℃, fully stirring the mixture at the same time, and soaking the mixture for 11-15 h at normal temperature after uniformly stirring the mixture to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 7.5-9 h in an air temperature environment of 88-92 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
Further, the copper nitrate is one or more of copper nitrate hexahydrate, copper nitrate trihydrate and anhydrous copper nitrate.
Further, the concentration of the copper nitrate solution in step S100 is 0.25mol/L, or 0.5mol/L, or 1mol/L, or 1.5mol/L, or 2 mol/L.
Further, the dipping time in step S200 was 12 hours.
Further, in step S300, the gas temperature environment is 90 ℃, and the activation time is 8 hours.
The invention also aims to provide a sulfur dioxide adsorbing material prepared by any one of the preparation methods.
Has the advantages that: the sulfur dioxide adsorbing material and the preparation method thereof are combined with the activated carbon as the raw material of the adsorbing material, and the preparation method thereof is provided, so that the adsorbing efficiency and the adsorbing capacity of the adsorbing material are remarkably improved.
Drawings
FIG. 1 is a graph of the adsorption breakthrough of activated carbon prepared from copper nitrate solutions of different concentrations in various examples of the invention.
FIG. 2 is a graph showing the adsorption capacity of activated carbon prepared from copper nitrate solutions of different concentrations in various examples of the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
example one
A preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing a copper nitrate solution by using 6.04g of copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 0.25mol/L, and the volume of the formed copper nitrate solution is 100 ml;
s200, taking 100ml of the copper nitrate solution obtained in the previous step, adding 50g of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 95 ℃, fully stirring the mixture at the same time, and soaking the mixture for 12 hours at normal temperature after the mixture is uniformly stirred to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 8 hours in an air temperature environment of 90 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
Example two
A preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing 12.08g of copper nitrate and plasma water into a copper nitrate solution, wherein the concentration of the formed copper nitrate solution is 0.5mol/L, and the volume of the formed copper nitrate solution is 100 ml;
s200, taking 100ml of the copper nitrate solution obtained in the previous step, adding 50g of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 95 ℃, fully stirring the mixture at the same time, and soaking the mixture for 12 hours at normal temperature after the mixture is uniformly stirred to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 8 hours in an air temperature environment of 90 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
EXAMPLE III
A preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing a copper nitrate solution by using 24.16g of copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 1mol/L, and the volume of the formed copper nitrate solution is 100 ml;
s200, taking 100ml of the copper nitrate solution obtained in the previous step, adding 50g of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 95 ℃, fully stirring the mixture at the same time, and soaking the mixture for 12 hours at normal temperature after the mixture is uniformly stirred to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 8 hours in an air temperature environment of 90 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
Example four
A preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing a copper nitrate solution by using 36.24g of copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 1.5mol/L, and the volume of the formed copper nitrate solution is 100 ml;
s200, taking 100ml of the copper nitrate solution obtained in the previous step, adding 50g of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 95 ℃, fully stirring the mixture at the same time, and soaking the mixture for 12 hours at normal temperature after the mixture is uniformly stirred to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 8 hours in an air temperature environment of 90 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
EXAMPLE five
A preparation method of a sulfur dioxide adsorbing material comprises the following steps:
s100, preparing 48.32g of copper nitrate and plasma water into a copper nitrate solution, wherein the concentration of the formed copper nitrate solution is 2mol/L, and the volume of the formed copper nitrate solution is 100 ml;
s200, taking 100ml of the copper nitrate solution obtained in the previous step, adding 50g of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 95 ℃, fully stirring the mixture at the same time, and soaking the mixture for 12 hours at normal temperature after the mixture is uniformly stirred to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 8 hours in an air temperature environment of 90 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
In order to compare the six examples, according to the above method, 0mol/L copper nitrate solution was set and the adsorption material was adjusted by adding activated carbon.
The comparative results are given in the following table:
sample piece Adsorption breakthrough time, min Adsorption capacity, mg/g
Control group 23 30.3
Example one 53 66.3
Example two 109 168.3
EXAMPLE III 102 162.7
Example four 73 131.9
EXAMPLE five 48 117.6
The adsorption breakthrough curves of activated carbon prepared from copper nitrate solutions of different concentrations are shown in fig. 1.
The adsorption capacity of activated carbon prepared from copper nitrate solutions of different concentrations is shown in fig. 2.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations can be devised by those skilled in the art in light of the above teachings. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (6)

1. The preparation method of the sulfur dioxide adsorbing material is characterized by comprising the following steps of:
s100, preparing copper nitrate solution by using copper nitrate and plasma water, wherein the concentration of the formed copper nitrate solution is 0.25-2 mol/L;
s200, taking 100 parts of copper nitrate solution obtained in the previous step in proportion, adding 50 parts of coconut shell activated carbon into the copper nitrate solution, heating the mixture in a water bath with the water temperature of 93-96 ℃, fully stirring the mixture at the same time, and soaking the mixture for 11-15 h at normal temperature after uniformly stirring the mixture to complete modification;
s300, filtering out a solution from the mixture impregnated in the previous step, and then putting the modified activated carbon into an air-blowing drying oven to activate for 7.5-9 h in an air temperature environment of 88-92 ℃ to complete activation;
s400, screening the activated carbon in the previous step by using a 200-mesh sieve, removing the activated carbon with small granularity, and reserving the activated carbon with large granularity as an adsorption material.
2. The method of claim 1 for producing a sulfur dioxide sorbent material, wherein: the copper nitrate is one or more of copper nitrate hexahydrate, copper nitrate trihydrate and anhydrous copper nitrate.
3. The method of claim 1 for producing a sulfur dioxide sorbent material, wherein: the concentration of the copper nitrate solution in step S100 is 0.25mol/L, 0.5mol/L, 1mol/L, 1.5mol/L or 2 mol/L.
4. The method of claim 1 for producing a sulfur dioxide sorbent material, wherein: the dipping time in step S200 was 12 hours.
5. The method of claim 1 for producing a sulfur dioxide sorbent material, wherein: in step S300, the gas temperature environment is 90 ℃, and the activation time is 8 h.
6. A sulfur dioxide adsorbent material characterized by being produced by the production method according to any one of claims 1 to 5.
CN202110719360.7A 2021-06-28 2021-06-28 Sulfur dioxide adsorption material and preparation method thereof Pending CN113522234A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101804325A (en) * 2010-04-22 2010-08-18 上海化工研究院 Preparation method of modified activated carbon adsorption desulfurizing agent
CN102059094A (en) * 2010-11-22 2011-05-18 山西新华化工有限责任公司 Preparation method of sulfur-removal activated carbon containing copper
CN105903324A (en) * 2016-05-18 2016-08-31 天津普瑞特净化技术有限公司 Copper oxide loaded active carbon desulfurizing agent and preparation process thereof
CN106423063A (en) * 2016-11-07 2017-02-22 江苏大学 Modified activated carbon, modifying method and application of modified activated carbon
CN110371974A (en) * 2019-08-21 2019-10-25 福建省鑫森炭业股份有限公司 Active carbon and preparation method thereof for removing hydrogen sulfide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101804325A (en) * 2010-04-22 2010-08-18 上海化工研究院 Preparation method of modified activated carbon adsorption desulfurizing agent
CN102059094A (en) * 2010-11-22 2011-05-18 山西新华化工有限责任公司 Preparation method of sulfur-removal activated carbon containing copper
CN105903324A (en) * 2016-05-18 2016-08-31 天津普瑞特净化技术有限公司 Copper oxide loaded active carbon desulfurizing agent and preparation process thereof
CN106423063A (en) * 2016-11-07 2017-02-22 江苏大学 Modified activated carbon, modifying method and application of modified activated carbon
CN110371974A (en) * 2019-08-21 2019-10-25 福建省鑫森炭业股份有限公司 Active carbon and preparation method thereof for removing hydrogen sulfide

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Title
孙威: ""活性炭吸附脱硫影响因素的实验研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
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Application publication date: 20211022