CN111135785A - Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof - Google Patents
Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof Download PDFInfo
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- CN111135785A CN111135785A CN202010011954.8A CN202010011954A CN111135785A CN 111135785 A CN111135785 A CN 111135785A CN 202010011954 A CN202010011954 A CN 202010011954A CN 111135785 A CN111135785 A CN 111135785A
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 44
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003463 adsorbent Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000002505 iron Chemical class 0.000 title claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 238000005470 impregnation Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003607 modifier Substances 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 26
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003546 flue gas Substances 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- 230000003213 activating effect Effects 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000013543 active substance Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 16
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000007602 hot air drying Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 208000000453 Skin Neoplasms Diseases 0.000 description 1
- 150000001495 arsenic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940093920 gynecological arsenic compound Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 201000005202 lung cancer Diseases 0.000 description 1
- 208000020816 lung neoplasm Diseases 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 201000000849 skin cancer Diseases 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/02—Separation 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/55—Compounds of silicon, phosphorus, germanium or arsenic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a gas-phase arsenic adsorbent and a preparation method and application thereof. Relates to an adsorbing material, a preparation method and application thereof, in particular to a method for preparing an adsorbent by solution impregnation for removing gas-phase arsenic. The gas-phase dearsenization adsorbent is finally obtained by taking activated alumina as a carrier, Mn salt and Ce salt as modifiers, loading ferric salt active substances by using an impregnation method, and drying by hot air and activating and roasting. The arsenic adsorbent provided by the invention is mainly applied to adsorption and removal of gas-phase arsenic in flue gas, and a gas-phase arsenic adsorption experiment proves that the introduction of the adsorbent greatly reduces the content of the gas-phase arsenic in the flue gas, and the trapping efficiency of the gas-phase arsenic is high.
Description
Technical Field
The invention relates to an adsorption material, a preparation method and application thereof, in particular to an iron-based and modified iron-based adsorbent prepared by an ultrasonic-assisted impregnation method and used for removing gas-phase arsenic.
Background
Arsenic is one of the most common and most harmful substances causing human carcinogenesis in the environment, all arsenic compounds are toxic, and can cause cell poisoning and capillary poisoning after long-term contact, and lung cancer, skin cancer and the like can be caused. Currently, the atmospheric emission of industrial arsenic is about 195.0 t/year, and the emission increases year by year as human activities increase. With the increasing attention of people to environmental protection and the stricter environmental regulations, the emission control of heavy metal arsenic in industrial flue gas has attracted wide attention at home and abroad.
The solid adsorbent is considered to be one of effective measures for gas phase heavy metal adsorption, and has wide application prospect in the aspect of removing arsenic-containing compounds in flue gas due to the advantages of large treatment capacity, high arsenic removal depth, high adaptability to various arsenide and the like.
For a long time, people pay attention to adsorption and removal of arsenic in water, for example, chinese patent CN 102941057a (application No. 201210450827.3) discloses a magnetic composite adsorbent for removing inorganic trivalent arsenic in water; chinese patent CN 101176840a (application No. 200610114389.8) discloses a method for preparing a de-arsenic adsorbent by modifying red mud with iron salt, which is used as a de-arsenic material for wastewater and drinking water.
However, the attention on the removal of gas-phase arsenic in industrial production flue gas is insufficient, no adsorbent for gas-phase arsenic exists at present, and research and development work on related gas-phase arsenic adsorbents is not carried out.
Disclosure of Invention
The invention aims to prepare a modified iron-based adsorption material by adopting an ultrasonic-assisted impregnation method, and apply the modified iron-based adsorption material to remove gas-phase arsenic.
The object of the invention can be achieved by the following measures:
(1) preparing a trivalent ferric salt serving as a precursor, using citric acid as a dispersing agent, using Mn salt/Ce salt as a modifier, and using a sodium hydroxide solution to adjust the pH of an impregnation solution to about 8 to obtain an impregnation solution; active alumina particles are used as an adsorbent carrier, and ultrasonic impregnation is carried out at a certain temperature.
(2) And (3) carrying out suction filtration on the impregnated carrier and the impregnating solution to be dried completely, and drying and washing the filtered sample with deionized water.
(3) And taking out the washed sample for roasting treatment to obtain the modified iron-based gas-phase arsenic adsorbent.
The preparation method of the gas-phase arsenic adsorbent provided by the invention has the beneficial effects that: the method is used for adsorption treatment of gas-phase arsenic in arsenic-containing flue gas, so that the content of the gas-phase arsenic in the flue gas is greatly reduced, the preparation method of the adsorbent is simple, the trapping efficiency of the gas-phase arsenic in the flue gas is high, and the method is easy to popularize on an industrial scale.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
The starting materials are commercially available from the open literature unless otherwise specified. The method is a conventional method unless otherwise specified.
Example 1:
the granular activated alumina carrier is subjected to alcohol washing to remove impurities on the surface of the carrier, and the carrier after the alcohol washing is subjected to hot air drying at 150 ℃ for 3 hours. Preparing 50 wt.% ferric nitrate solution, adding citric acid dispersant according to the mass ratio of 1: 0.01 of ferric nitrate and citric acid, adding modifier manganese nitrate according to the molar ratio of 2%, and heating and stirring the solution for 20 minutes in a water bath environment at 50 ℃. 20g of activated alumina carrier is weighed and poured into 80mL of solution for ultrasonic dipping, the water temperature of an ultrasonic oscillator is set to be 30 ℃, the ultrasonic power is 100%, and the activated alumina carrier is taken out after 4h of dipping. The impregnated sample was poured into a buchner funnel and filtered to dryness. And (3) placing the sample which is completely filtered and dried in a hot air drying box for primary drying, wherein the drying condition is 115 ℃ for 12 hours. And taking out the dried sample for roasting and activating, wherein the specific parameters are 700 ℃ and 4 h.
The resulting adsorbent sample was designated a 1.
Example 2:
the granular activated alumina carrier is subjected to alcohol washing to remove impurities on the surface of the carrier, and the carrier after the alcohol washing is subjected to hot air drying at 150 ℃ for 3 hours. Preparing 35 wt.% ferric chloride solution, adding citric acid dispersant according to the mass ratio of ferric nitrate to citric acid of 1: 0.01, adding modifier manganese nitrate according to the molar ratio of 7%, and heating and stirring the solution for 20 minutes in a water bath environment at 50 ℃. 20g of activated alumina carrier is weighed and poured into 80mL of solution for ultrasonic dipping, the water temperature of an ultrasonic oscillator is set to be 30 ℃, the ultrasonic power is 100%, and the activated alumina carrier is taken out after 4h of dipping. The impregnated sample was poured into a buchner funnel and filtered to dryness. And (3) placing the sample which is completely filtered and dried in a hot air drying box for primary drying, wherein the drying condition is 115 ℃ for 12 hours. And taking out the dried sample for roasting and activating, wherein the specific parameters are 700 ℃ and 4 h.
The resulting adsorbent sample was designated a 2.
Example 3:
the granular activated alumina carrier is subjected to alcohol washing to remove impurities on the surface of the carrier, and the carrier after the alcohol washing is subjected to hot air drying at 150 ℃ for 3 hours. Preparing 25 wt.% ferric nitrate solution, adding citric acid dispersant according to the mass ratio of 1: 0.01 of ferric nitrate and citric acid, adding modifying agent cerous nitrate according to the molar ratio of 2%, and heating and stirring the solution for 20 minutes in a water bath environment at 50 ℃. 20g of activated alumina carrier is weighed and poured into 80mL of solution for ultrasonic dipping, the water temperature of an ultrasonic oscillator is set to be 30 ℃, the ultrasonic power is 100%, and the activated alumina carrier is taken out after 4h of dipping. The impregnated sample was poured into a buchner funnel and filtered to dryness. And (3) placing the sample which is completely filtered and dried in a hot air drying box for primary drying, wherein the drying condition is 115 ℃ for 12 hours. And taking out the dried sample for roasting and activating, wherein the specific parameters are 700 ℃ and 4 h.
The resulting adsorbent sample was designated a 3.
Test examples 1 to 3:
150mg of the adsorbents A1, A2 and A3 prepared in the above examples were put in a fixed bed reactor to perform a gas phase arsenic adsorption experiment. Setting the content of gas-phase arsenic to be 100ppb, the flow rate of simulated flue gas to be 500mL/min, the adsorption time to be 120min and the adsorption temperature to be 300 ℃. The adsorbed sample was pretreated according to the national standard method, and the obtained sample was subjected to an arsenic content test using an atomic fluorescence spectrophotometer (available from Millennium Excalibur, PSA, england) to finally measure the adsorption efficiency of the adsorbent.
The adsorption results are shown in Table 1.
Test examples 4 to 6:
150mg of the adsorbents A1, A2 and A3 prepared in the above examples were put in a fixed bed reactor to perform a gas phase arsenic adsorption experiment. The gas-phase arsenic content is set to be 200ppb, the flow rate of simulated flue gas is 500mL/min, the adsorption time is 120min, and the adsorption temperature is set to be 500 ℃. Pretreating the adsorbed sample according to a national standard method, testing the arsenic content of the obtained sample by using an atomic fluorescence spectrophotometer, and finally measuring the adsorption efficiency of the adsorbent.
The adsorption results are shown in Table 1.
Test examples 7 to 9:
150mg of the adsorbents A1, A2 and A3 prepared in the above examples were put in a fixed bed reactor to perform a gas phase arsenic adsorption experiment. Setting the content of gas-phase arsenic to 300ppb, the flow rate of simulated flue gas to 500mL/min, the adsorption time to 120min and the adsorption temperature to 700 ℃. Pretreating the adsorbed sample according to a national standard method, testing the arsenic content of the obtained sample by using an atomic fluorescence spectrophotometer, and finally measuring the adsorption efficiency of the adsorbent.
The adsorption results are shown in Table 1.
TABLE 1
| Example numbering | Sorbent numbering | Adsorption efficiency (%) |
| Test example 1 | A1 | 65 |
| Test example 2 | A2 | 51 |
| Test example 3 | A3 | 73 |
| Test example 4 | A1 | 76 |
| Test example 5 | A2 | 60 |
| Test example 6 | A3 | 85 |
| Test example 7 | A1 | 81 |
| Test example 8 | A2 | 65 |
| Test example 9 | A3 | 93 |
As can be seen from the test examples in table 1, the adsorbent prepared in example 3 has relatively high adsorption efficiency for arsenic in the gas phase compared to the adsorbents prepared in examples 1 and 2, and the temperature rise for the adsorbents prepared in examples 1, 2 and 3 promotes adsorption of arsenic in the gas phase.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, various simple combination modifications can be made to the technical solution of the invention, for example, adjusting the calcination temperature for preparing the adsorbent, adjusting the solution concentration, etc. These simple modifications should be considered as the disclosure of the present invention, and all fall into the scope of the present invention.
Claims (2)
1. The arsenic removal adsorbent and the preparation method and the application thereof are characterized in that: trivalent iron salt is used as a precursor, Mn salt and Ce salt are used as modifiers, and active oxide is used as an adsorbent carrier. The preparation method comprises the following three steps:
(1) preparing a trivalent ferric salt serving as a precursor, using citric acid as a dispersing agent, using Mn salt/Ce salt as a modifier, and using a sodium hydroxide solution to adjust the pH of an impregnation solution to about 8 to obtain an impregnation solution; active alumina particles are used as an adsorbent carrier, and ultrasonic impregnation is carried out at a certain temperature.
(2) And (3) carrying out suction filtration on the impregnated carrier and the impregnating solution to be dried completely, and drying and washing the filtered sample with deionized water.
(3) And taking out the washed sample for roasting treatment to obtain the modified iron-based gas-phase arsenic adsorbent.
2. The arsenic removal sorbent of claim 1, wherein the product is used for gas phase arsenic removal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010011954.8A CN111135785A (en) | 2020-01-07 | 2020-01-07 | Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof |
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| CN202010011954.8A CN111135785A (en) | 2020-01-07 | 2020-01-07 | Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof |
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| CN202010011954.8A Pending CN111135785A (en) | 2020-01-07 | 2020-01-07 | Modified iron-based gas-phase arsenic adsorbent and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115646431A (en) * | 2022-10-24 | 2023-01-31 | 中南大学 | Gaseous arsenic adsorption material and preparation and application thereof |
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| US20030116504A1 (en) * | 2001-07-24 | 2003-06-26 | Vempati Rajan K. | Absorbent for arsenic species and method of treating arsenic-contaminated waters |
| CN106669721A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Iron-based supported catalyst and preparation method thereof |
| CN108499516A (en) * | 2018-04-03 | 2018-09-07 | 中国神华能源股份有限公司 | Support type arsenic adsorbent and its preparation method and application and the method for arsenic removing |
| CN109078608A (en) * | 2018-08-31 | 2018-12-25 | 中国环境科学研究院 | Arsenic-removing adsorption agent and preparation method and application based on iron modified activated aluminum oxide |
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| CN110327874A (en) * | 2019-07-04 | 2019-10-15 | 江西理工大学 | A kind of compound Fe-Ce oxide dearsenification adsorbent of core-shell structure and its preparation method and application |
-
2020
- 2020-01-07 CN CN202010011954.8A patent/CN111135785A/en active Pending
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Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115646431A (en) * | 2022-10-24 | 2023-01-31 | 中南大学 | Gaseous arsenic adsorption material and preparation and application thereof |
| CN115646431B (en) * | 2022-10-24 | 2024-01-26 | 中南大学 | Gaseous arsenic adsorbing material, preparation and application thereof |
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Application publication date: 20200512 |