CN109399726B - Preparation method of iron lanthanum oxide molecular sieve type purification material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000746 purification Methods 0.000 title claims abstract description 35
- GZHZIMFFZGAOGY-UHFFFAOYSA-N [O-2].[Fe+2].[La+3] Chemical compound [O-2].[Fe+2].[La+3] GZHZIMFFZGAOGY-UHFFFAOYSA-N 0.000 title claims abstract description 26
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 32
- NNLJGFCRHBKPPJ-UHFFFAOYSA-N iron lanthanum Chemical compound [Fe].[La] NNLJGFCRHBKPPJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 6
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 claims abstract description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 6
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims abstract description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims abstract description 6
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 16
- 239000011148 porous material Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 2
- 230000004913 activation Effects 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 8
- 238000005286 illumination Methods 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000003213 activating effect Effects 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- -1 tungsten halogen Chemical class 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
-
- 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
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- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- 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
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- 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
- B01J29/00—Catalysts comprising molecular sieves
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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Abstract
A preparation method of an iron lanthanum oxide molecular sieve type purification material belongs to the field of environment-friendly purification materials, and comprises the following steps: preparing a solution A from absolute ethyl alcohol, polyethylene glycol, hexadecyl trimethyl ammonium bromide and Span60, preparing a solution B from deionized water, lanthanum acetate, ferric trichloride, polyacrylamide and sodium dihydrogen phosphate, and mixing the solution A and the solution B to obtain an iron lanthanum precursor; carrying out hydrothermal reaction, filtering, drying and calcining on the iron lanthanum precursor to obtain a solid; and (3) treating the solid with a phosphoric acid solution, and drying to obtain the iron lanthanum oxide molecular sieve type purification material. The purifying material has large specific surface area and porous characteristic, can fully adsorb organic pollutants in water and air, and can rapidly and effectively decompose organic matters under illumination.
Description
Technical Field
The invention belongs to the field of environment-friendly purification materials, and particularly relates to a preparation method of an iron lanthanum oxide molecular sieve type purification material.
Background
Due to the wide use of various toxic and harmful artificially synthesized organic pollutants, more and more organic pollutants enter water, atmosphere and other global environments, and the pollutants in drinking water and indoor air cause great harm to human health, which has caused great concern to people. The environment-friendly purifying material is a functional material which can be used for purifying pollution, and the action mechanism of the environment-friendly purifying material comprises adsorption, filtration, flocculation, oxidation and the like. The most widely used environmental-friendly purification materials are various adsorbents which can adsorb and remove organic pollutants. However, such materials do not have a continuous purification capacity, and must be regenerated after saturation of adsorption, and the adsorbed organic substances are removed by a regeneration procedure to restore the adsorption capacity of the material. In order to make the environmental-friendly purification material have a longer service life, the environmental-friendly purification material needs to have the activity of decomposing organic pollutants, namely, the environmental-friendly purification material can adsorb and decompose organic matters at the same time, and the material has huge application prospects.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of an iron lanthanum oxide molecular sieve type purification material, which can be used for purifying organic pollutants in water and air. The purifying material can adsorb organic matter and degrade the organic matter under illumination, and is suitable for various water and air pollution purifying fields.
A preparation method of an iron lanthanum oxide molecular sieve type purification material comprises the following preparation steps.
Step 1: preparing iron lanthanum precursor.
(1) Adding 7-10 g of polyethylene glycol 20000, 1.5-2 g of hexadecyl trimethyl ammonium bromide and 3-5 g of emulsifier Span60 into 200mL of absolute ethyl alcohol, and stirring to form a solution A.
(2) Adding 8-11 g of lanthanum acetate, 12-15 g of ferric trichloride, 3-6 g of polyacrylamide with the molecular weight of 200 ten thousand and 3.5-4.5 g of sodium dihydrogen phosphate into 280mL of deionized water, and stirring to form a solution B.
(3) And mixing the solution A and the solution B to obtain the iron lanthanum precursor.
Step 2: and (5) carrying out hydrothermal forming.
And (3) moving the iron lanthanum precursor into a stainless steel hydrothermal reaction kettle, reacting for 60 hours at 260-270 ℃, cooling, filtering, and drying the obtained solid substance for 20 hours at 190 ℃ to obtain a solid substance A.
And step 3: and (4) calcining and crystallizing.
And calcining the solid A at 800-850 ℃ for 6h, and cooling to obtain a solid B.
And 4, step 4: and (4) activating.
Mixing the solid B with 700mL of 0.6mol/L phosphoric acid solution, heating to 85 ℃, preserving the temperature for 200min, filtering, and drying the obtained solid substance at 190 ℃ for 20h to obtain the iron lanthanum oxide molecular sieve type purification material.
The prepared iron lanthanum oxide molecular sieve type purification material has the following technical characteristics: pore size is 6-7 nm, and specific surface area is 520-760 m2Per g, pore volume of 0.5-0.6 cm3(ii) a bulk density of 0.9 to 1.0g/cm3。
Compared with the prior art, the preparation method of the iron lanthanum oxide molecular sieve type purification material has the advantages that: iron lanthanum oxide has photocatalytic purification activity, but the related materials prepared in general are not highly active due to lack of regular pore structure. The invention adopts a reasonable preparation process, takes iron lanthanum oxide as a basic framework composition, and forms a regular porous characteristic with a molecular sieve structure in the material. Fe-O-La forms a ring structure and forms a specific hollow cage structure by extending in a three-dimensional space. The opening size of the Fe-O-La ring is 6-7 nm. After the molecular sieve type structure is formed, the iron lanthanum oxide can fully adsorb organic pollutants in water and air, and can quickly and effectively decompose organic matters under illumination, so that the effect of continuously and quickly purifying the organic pollutants is achieved.
Detailed Description
Example 1.
A preparation method of an iron lanthanum oxide molecular sieve type purification material mainly comprises the following steps.
Step 1: preparing iron lanthanum precursor.
(1) To 200mL of absolute ethanol were added 7g of polyethylene glycol 20000, 1.5g of cetyltrimethylammonium bromide and 3g of emulsifier Span60, followed by stirring to obtain a solution A.
(2) 8g of lanthanum acetate, 12g of ferric trichloride, 3g of polyacrylamide with the molecular weight of 200 ten thousand and 3.5g of sodium dihydrogen phosphate are added into 280mL of deionized water, and stirred to form a solution B.
(3) And mixing the solution A and the solution B to obtain the iron lanthanum precursor.
Step 2: and (5) carrying out hydrothermal forming.
And (3) moving the iron lanthanum precursor into a stainless steel hydrothermal reaction kettle, reacting for 60h at 260 ℃, cooling, filtering, and drying the obtained solid substance for 20h at 190 ℃ to obtain a solid substance A.
And step 3: and (4) calcining and crystallizing.
Calcining the solid A at 800 ℃ for 6h, and cooling to obtain a solid B.
And 4, step 4: and (4) activating.
Mixing the solid B with 700mL of 0.6mol/L phosphoric acid solution, heating to 85 ℃, preserving the temperature for 200min, filtering, and drying the obtained solid substance at 190 ℃ for 20h to obtain the iron lanthanum oxide molecular sieve type purification material.
The prepared iron lanthanum oxide molecular sieve type purification material has the following technical characteristics: pore size 6nm and specific surface area 520m2G, pore volume 0.5cm3(g), bulk density 0.9g/cm3。
And (5) detecting the performance.
20mg of the purification material prepared in example 1 was added to 100mL of a methyl orange solution having a concentration of 10mg/L, and the mixture was stirred in the dark for 60min to determine the concentration of the methyl orange solution; the solution was then placed under a 150W tungsten halogen lamp and the methyl orange solution concentration was measured every 10 min. And calculating the adsorption rate and the photocatalytic degradation rate of the methyl orange on the purification material.
According to the measurement result, the equilibrium saturation adsorption rate of the methyl orange on the purification material is 6.5%. After irradiation under a halogen tungsten lamp, methyl orange generates photocatalytic degradation reaction on the purification material; after 30min of photocatalytic degradation reaction, the photocatalytic degradation rate of the methyl orange solution reaches 100%.
Example 2.
A preparation method of an iron lanthanum oxide molecular sieve type purification material mainly comprises the following steps.
Step 1: preparing iron lanthanum precursor.
(1) To 200mL of absolute ethanol were added 8.5g of polyethylene glycol 20000, 1.7g of cetyltrimethylammonium bromide and 4g of emulsifier Span60, followed by stirring to obtain a solution A.
(2) 9g of lanthanum acetate, 13g of ferric chloride, 4.5g of polyacrylamide with the molecular weight of 200 ten thousand and 4g of sodium dihydrogen phosphate are added into 280mL of deionized water, and stirred to form a solution B.
(3) And mixing the solution A and the solution B to obtain the iron lanthanum precursor.
Step 2: and (5) carrying out hydrothermal forming.
And (3) moving the iron lanthanum precursor into a stainless steel hydrothermal reaction kettle, reacting for 60h at 265 ℃, cooling, filtering, and drying the obtained solid substance for 20h at 190 ℃ to obtain a solid substance A.
And step 3: and (4) calcining and crystallizing.
The solid A was calcined at 820 ℃ for 6h and cooled to give solid B.
And 4, step 4: and (4) activating.
Mixing the solid B with 700mL of 0.6mol/L phosphoric acid solution, heating to 85 ℃, preserving the temperature for 200min, filtering, and drying the obtained solid substance at 190 ℃ for 20h to obtain the iron lanthanum oxide molecular sieve type purification material.
The prepared iron lanthanum oxide molecular sieve type purification material has the following technical characteristics: pore size 6nm, specific surface area 630m2G, pore volume 0.5cm3(g), bulk density 0.9g/cm3。
Example 3.
A preparation method of an iron lanthanum oxide molecular sieve type purification material mainly comprises the following steps.
Step 1: preparing iron lanthanum precursor.
(1) 10g of polyethylene glycol 20000, 2g of cetyltrimethylammonium bromide and 5g of emulsifier Span60 were added to 200mL of anhydrous ethanol, and stirred to form a solution A.
(2) 11g of lanthanum acetate, 15g of ferric trichloride, 6g of polyacrylamide with the molecular weight of 200 ten thousand and 4.5g of sodium dihydrogen phosphate are added into 280mL of deionized water, and stirred to form a solution B.
(3) And mixing the solution A and the solution B to obtain the iron lanthanum precursor.
Step 2: and (5) carrying out hydrothermal forming.
And (3) moving the iron lanthanum precursor into a stainless steel hydrothermal reaction kettle, reacting for 60h at 270 ℃, cooling, filtering, and drying the obtained solid substance for 20h at 190 ℃ to obtain a solid substance A.
And step 3: and (4) calcining and crystallizing.
Calcining the solid A at 850 ℃ for 6h, and cooling to obtain a solid B.
And 4, step 4: and (4) activating.
Mixing the solid B with 700mL of 0.6mol/L phosphoric acid solution, heating to 85 ℃, preserving the temperature for 200min, filtering, and drying the obtained solid substance at 190 ℃ for 20h to obtain the iron lanthanum oxide molecular sieve type purification material.
The prepared iron lanthanum oxide molecular sieve type purification material has the following technical characteristics: pore size 7nm, specific surface area 760m2G, pore volume 0.6cm3(g), bulk density 1.0g/cm3。
Claims (2)
1. The preparation method of the iron lanthanum oxide molecular sieve type purification material is characterized by comprising the following process steps:
step 1: preparation of iron lanthanum precursor
(1) Adding 7-10 g of polyethylene glycol 20000, 1.5-2 g of hexadecyl trimethyl ammonium bromide and 3-5 g of emulsifier Span60 into 200mL of absolute ethyl alcohol, and stirring to form a solution A;
(2) adding 8-11 g of lanthanum acetate, 12-15 g of ferric trichloride, 3-6 g of polyacrylamide with the molecular weight of 200 ten thousand and 3.5-4.5 g of sodium dihydrogen phosphate into 280mL of deionized water, and stirring to form a solution B;
(3) mixing the solution A and the solution B to obtain an iron lanthanum precursor;
step 2: hydrothermal forming
Moving the iron lanthanum precursor into a stainless steel hydrothermal reaction kettle, reacting for 60 hours at 260-270 ℃, cooling, filtering, and drying the obtained solid substance for 20 hours at 190 ℃ to obtain a solid substance A;
and step 3: calcined crystals
Calcining the solid A at 800-850 ℃ for 6h, and cooling to obtain a solid B;
and 4, step 4: activation of
Mixing the solid B with 700mL of 0.6mol/L phosphoric acid solution, heating to 85 ℃, preserving the temperature for 200min, filtering, and drying the obtained solid substance at 190 ℃ for 20h to obtain the iron lanthanum oxide molecular sieve type purification material.
2. The method for preparing iron lanthanum oxide molecular sieve type purification material according to claim 1, wherein the prepared iron lanthanum oxide molecular sieve type purification material has the following technical characteristics: pore size is 6-7 nm, and specific surface area is 520-760 m2Per g, pore volume of 0.5-0.6 cm3(ii) a bulk density of 0.9 to 1.0g/cm3。
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CN105600833B (en) * | 2015-10-15 | 2017-07-07 | 齐鲁工业大学 | A kind of spherical mesoporous iron oxide and preparation method thereof |
CN105688825B (en) * | 2016-04-21 | 2017-11-14 | 济南大学 | A kind of magnetic adsorbent preparation method and application based on ferrous metals organic framework material |
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