CN111957985A - Method for green synthesis of nano-iron by using ilex latifolia and application - Google Patents
Method for green synthesis of nano-iron by using ilex latifolia and application Download PDFInfo
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- CN111957985A CN111957985A CN202010820554.1A CN202010820554A CN111957985A CN 111957985 A CN111957985 A CN 111957985A CN 202010820554 A CN202010820554 A CN 202010820554A CN 111957985 A CN111957985 A CN 111957985A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 107
- 244000078118 Ilex latifolia Species 0.000 title claims abstract description 65
- 235000008706 Ilex latifolia Nutrition 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 34
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 33
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- 239000005017 polysaccharide Substances 0.000 claims abstract description 50
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000000126 substance Substances 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 150000002505 iron Chemical class 0.000 claims abstract description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 59
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 239000007787 solid Substances 0.000 claims description 34
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
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- 235000013580 sausages Nutrition 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
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- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 9
- 229960000907 methylthioninium chloride Drugs 0.000 description 9
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- 229910052603 melanterite Inorganic materials 0.000 description 7
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
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- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
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- 241000196324 Embryophyta Species 0.000 description 1
- 235000003325 Ilex Nutrition 0.000 description 1
- 241000209035 Ilex Species 0.000 description 1
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- 241000422846 Sequoiadendron giganteum Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
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- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/23—
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/327—Polyaromatic Hydrocarbons [PAH's]
Abstract
The invention relates to a method for green synthesis of nano-iron by using ilex latifolia, which can regulate and control green synthesis of a high-reactivity nano-iron material and improve the reaction activity of the green synthesis of the nano-iron, and comprises the following specific steps: (1) extracting polysaccharide substances in the ilex latifolia to obtain a polysaccharide extracting solution; (2) polysaccharide solution is used as a reducing agent to reduce iron salt to prepare green synthetic nano iron.
Description
Technical Field
The invention belongs to the technical field of environmental pollution treatment materials, relates to a method for green synthesis of nano-iron by using plant extract and application thereof, and particularly relates to a method for green synthesis of nano-iron by using ilex latifolia and application thereof.
Background
With the rapid development of nanotechnology, the nano iron material is used for removing environmental pollutants, shows excellent performance, and draws great attention. The nano iron material is mainly iron and oxides thereof, and recently also comprises a nano iron material doped with dissimilar metals, the nano iron materials can provide a larger specific surface area and more active sites, and part of the nano iron material has excellent biocompatibility. The traditional synthetic method comprises a physical method and a chemical method, and the physical method comprises a high-energy ball milling method and the like; the preparation method is characterized in that the nano zero-valent iron is prepared by a chemical method, and iron salt and the like are effectively reduced mainly by a chemical reducing agent, so that nano iron particles can be obtained, and the method comprises a solid phase reduction method; the physical and chemical synthesis methods are mature day by day, and have obvious promotion effect on the development of the nanotechnology, but the synthesis process has more defects, namely higher energy consumption level, expensive unit preparation cost, easy secondary pollution and the like. The nano iron obtained by the conventional method has already been researched and founded for restoring the environmental pollution, but the nano iron materials are often agglomerated during synthesis to form a chain structure, so that the specific surface area of the nano iron materials is reduced; the nano iron particles prepared by the conventional method are very easy to oxidize in the air, are only limited to laboratory research and are rarely applied in engineering.
The synthesis of nano-iron materials by plant extract is gradually developing into a mature method, which can not only reduce the cost and energy consumption, but also reduce the use of chemical reagents and protect the environment. The green synthesized nano-iron material not only has a certain space shape to prevent the nano-iron material from agglomerating, but also can protect active sites on nano-particles. For example, the extract of tea leaves, grape leaves and the like plays a role of a reducing agent and a stabilizing agent in the preparation of nano metal, tea polyphenol in the tea leaves can reduce iron ions to realize the preparation of nano zero-valent iron, and the nano iron is used as a catalyst in a Fenton reaction to realize the effective degradation of bromothymol blue.
The Ilex latifolia (with the scientific name of Ilex latifolia Thunb.) is a evergreen big tree, the leaf is thick and leather, and is oblong or oval, and a pseudo-cone inflorescence consisting of a polypodium is grown in the axilla of a biennial branch without total stems; the flower is light yellow and green, the fruit is spherical, the fruit is red when ripe, the flowering phase is 4 months, and the fruit phase is 9-10 months. The ilex latifolia is grown in a slope evergreen broad-leaved forest, irrigation bush or bamboo forest with the elevation of 250-1500 m, is distributed in various provinces and Fujian provinces in Japan and the lower reaches of Yangtze river in China, and has rich resources in the Fujian province.
Although the research on the preparation of nano-iron by using plants at present deduces components with reduction effect in plant extract, it is not clear which components in the plant extract act on iron ions to reduce the iron ions into nano-iron, and which components in the extract cover the surface of the nano-iron to better maintain the activity of the iron ions, so that the quality and the reactivity of the nano-iron prepared by using the plant extract have high randomness and are unstable, and the nano-iron cannot be well controlled and produced in quantity.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for green synthesis of nano-iron by using ilex latifolia and application thereof, which can regulate and control green synthesis of a high-reactivity nano-iron material, and further improve the reaction activity of the green synthesis of nano-iron.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) extracting polysaccharide substances in the ilex latifolia to obtain a polysaccharide extracting solution;
(2) polysaccharide solution is used as a reducing agent to reduce iron salt to prepare green synthetic nano iron.
Further, the step (1) of preparing the polysaccharide extract comprises the following specific steps:
a1, weighing 30-60 g of dry and ground ilex latifolia powder, adding 0.8-1L of distilled water, heating in a water bath at 80-90 ℃ for 1-1.5 h, and performing suction filtration for later use;
a2, separating 400-500 mL of filtrate, extracting with ethyl acetate or ether for multiple times for 2-4 min respectively, and combining aqueous phase liquid obtained after multiple ethyl acetate or ether extractions to serve as ilex latifolia polysaccharide extracting solution for later use.
Further, in the step A2, the ethyl acetate or the ethyl ether is extracted from the filtrate for 3 times, and each time, 100-200 mL of ethyl acetate or ethyl ether is used for extraction.
Further, the step (1) of preparing the polysaccharide extract comprises the following specific steps:
b1, weighing 30-60 g of dried and ground ilex latifolia powder, and leaching for at least 2 times with 250-500 mL of 80% ethanol for 1-2 hours each time;
b2, heating the residual residues in a water bath at the temperature of 80-90 ℃ after leaching, and respectively extracting with deionized water for at least 3 times, wherein each extraction needs 2-2.5 hours;
b3, combining the multiple extracting solutions, transferring the extracting solutions into a rotary evaporator, concentrating under a reduced pressure condition to enable the extracting solutions to be in a final crystallization moisture-free state, filling the concentrated solution into a sausage casing, soaking the concentrated solution into pure water for 2-3 days, dissolving the concentrated solution again, and decolorizing the concentrated solution through S-8 macroporous resin;
b4, adding 3 times of volume of absolute ethyl alcohol into the extract obtained in the step B3, continuously stirring the mixture overnight, then carrying out centrifugal treatment, and drying the obtained precipitate; adding 1-1.5L of deionized water into the dried precipitate to dissolve the precipitate to prepare ilex latifolia polysaccharide extracting solution;
further, the specific steps for preparing the green synthetic nano-iron in the step (2) are as follows:
s1, preparing 0.10mol/L FeSO4·7H2Adding O solution slowly dropwise into the polysaccharide extract of ilex latifolia under nitrogen protection, stirring, and adding FeSO4Continuously stirring for 20-30 min after the solution is dripped until the reaction is complete;
s2, filtering the reaction liquid obtained in the step S1, washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at the temperature of 60-70 ℃ for drying overnight, taking out the dried solid after drying, and smashing and grinding the dried solid to obtain the product of the nano iron particles.
Further, in the step S1, the ilex latifolia polysaccharide extract and FeSO4·7H2The volume ratio of the O solution is 5: 1.
The invention also provides application of the nano-iron prepared by the method for green synthesis of nano-iron by using the ilex latifolia in repairing water and soil environments compounded by heavy metals and polycyclic aromatic hydrocarbons.
The invention has the beneficial effects that:
1. the invention provides a method for green synthesis of nano-iron by using ilex latifolia, which researches and extracts polysaccharide in ilex latifolia as a main reducing agent to reduce ferrous ions to prepare nano-iron particles, wherein the yield is 62%, and Fe is2+Is electrostatically attracted by negatively charged oxygen atoms (e.g., hydroxyl, etheroxy, etc.) on the polysaccharide, followed by Fe2+Reducing with aldehyde group on polysaccharide to generate Fe0The oxidation of aldehyde groups to carboxyl groups is continuously carried out around polysaccharide molecules, Fe0The crystal nucleus slowly grows into nano iron particles, polysaccharide substances and Fe2+The activity of the nano-iron generated by the reaction is higher, mainly because the polysaccharide substance is macromolecule, the nano-iron has larger molecular weight, more complex spatial structure and more effective electron transfer mode, so that the nano-iron synthesized by the polysaccharide substance has higher reaction activity, and further the stable production of the nano-iron synthesized by green ilex latifolia is ensuredThe reaction activity of the green synthesized nano iron is also improved.
2. The method for green synthesis of nano-iron by using ilex latifolia thumb provided by the invention not only ensures the yield and the reaction activity of green synthesis of nano-iron by using polysaccharide substances as main reducing agents, but also ensures that partial effective components such as polyphenol and flavone in ilex latifolia thumb participate in reduction of Fe in actual reaction2+The active site for generating the nano-particles is masked as a masking agent, so that the defects of easy agglomeration, easy oxidation and the like of nano-iron can be effectively overcome, and the prepared nano-iron particles have good stability.
Drawings
FIG. 1 is a schematic diagram of green synthesis of nano-iron according to the present invention;
FIG. 2 is a TEM scanning image of green synthesized nano-iron of the present invention;
FIG. 3 is a schematic diagram showing the comparison of the reactivity ratios of green synthesized nano-iron prepared according to example 1, comparative example 1 and comparative example 2;
FIG. 4 is a schematic diagram showing the removal rate of heavy metals in green synthesized nano-iron treated coal leachate according to the present invention;
FIG. 5 is a schematic diagram of the removal rate of polycyclic aromatic hydrocarbons in the green synthesized nano-iron catalytic Fenton reaction degraded soil.
Detailed Description
The invention will be further described with reference to preferred embodiments.
Example 1
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 60g of dry and ground ilex latifolia powder, adding 1L of distilled water, heating in water bath at 80 ℃ for 1h, and performing suction filtration for later use;
(2) respectively extracting 500mL of filtrate for 4min by ethyl acetate for multiple times, extracting for 4min by 200mL of ethyl acetate for the first time, extracting for 4min by 200mL of ethyl acetate for the second time, extracting for 4min by 100mL of ethyl acetate for the third time, combining aqueous phase liquid obtained after three-time extraction as ilex latifolia polysaccharide extracting solution, and keeping organic phase extracted by ethyl acetate for later use;
(3) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 200mLFeSO4·7H2Slowly dripping O solution into 1L of ilex latifolia polysaccharide extractive solution, stirring, and adding FeSO4Continuously stirring the solution for 20min after the solution is dropwise added until the reaction is complete;
(4) and (4) filtering the reaction liquid obtained in the step (3), washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at 60 ℃ for drying overnight, taking out the solid after drying, mashing and grinding the solid to obtain the product of nano iron particles.
Example 2
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 30g of dried and ground ilex latifolia powder, adding 0.8L of distilled water, heating in water bath at 90 ℃ for 1.5h, and performing suction filtration for later use;
(2) taking 400mL of filtrate, extracting with ethyl acetate for 2min for multiple times, extracting with 200mL of ethyl acetate for 2min for the first time, extracting with 100mL of ethyl acetate for 2min for the second time, extracting with 100mL of ethyl acetate for 2min for the third time, and combining aqueous phase liquids obtained after three-time extraction to serve as ilex latifolia polysaccharide extracting solution for later use;
(3) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 100mLFeSO4·7H2Slowly dripping O solution into 500mL ilex latifolia polysaccharide extract, stirring, and FeSO4Continuously stirring the solution for 25min after the solution is dropwise added until the reaction is complete;
(4) and (4) filtering the reaction liquid obtained in the step (3), washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at 70 ℃ for drying overnight, taking out the solid after drying, mashing and grinding the solid to obtain the product of nano iron particles.
Example 3
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 50g of dried and ground ilex latifolia powder, adding 1L of distilled water, heating in water bath at 80 ℃ for 1.5h, and performing suction filtration for later use;
(2) respectively extracting 500mL of filtrate with diethyl ether for 3min, extracting with 200mL of diethyl ether for 3min for the first time, extracting with 200mL of diethyl ether for 3min for the second time, extracting with 100mL of diethyl ether for 3min for the third time, and mixing the water phase solutions obtained after three-time extraction to obtain ilex latifolia polysaccharide extract;
(3) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 200mLFeSO4·7H2Slowly dripping O solution into 1L of ilex latifolia polysaccharide extractive solution, stirring, and adding FeSO4Continuously stirring the solution for 30min after the dropwise addition is finished until the reaction is complete;
(4) and (4) filtering the reaction liquid obtained in the step (3), washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at 60 ℃ for drying overnight, taking out the solid after drying, mashing and grinding the solid to obtain the product of nano iron particles.
Example 4
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 60g of dried and ground ilex latifolia powder, and respectively leaching with 500mL of 80% ethanol for 2 times, each time for 1 h;
(2) heating the residue in water bath at 80 deg.C, and extracting with deionized water for 2 hr for 3 times;
(3) mixing the extractive solutions, transferring into rotary evaporator, concentrating under reduced pressure to obtain crystal without water, loading into sausage casing, soaking in pure water for 3 days, dissolving, and decolorizing with S-8 macroporous resin;
(4) b3, adding 3 times of anhydrous ethanol, continuously stirring overnight, centrifuging, and drying the obtained precipitate; adding 1L deionized water into the dried precipitate to dissolve the precipitate to obtain ilex latifolia polysaccharide extractive solution;
(5) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 200mLFeSO4·7H2Slowly dripping O solution into 1L of ilex latifolia polysaccharide extractive solution, stirring, and adding FeSO4Continuously stirring the solution for 20min after the solution is dropwise added until the reaction is complete;
(6) and (4) filtering the reaction liquid obtained after the step S1, washing the rest solid for multiple times by using ethanol, transferring the solid into a vacuum drying oven at 60 ℃ for drying overnight, taking out the solid after the drying is finished, and smashing and grinding the solid to obtain the product of the nano iron particles.
Example 5
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 30g of dried and ground ilex latifolia powder, and respectively leaching with 250mL of 80% ethanol for 3 times, each time for 2 h;
(2) heating the residue in water bath at 90 deg.C, extracting with deionized water for 3 times (2.5 hr each time);
(3) mixing the extractive solutions, transferring into rotary evaporator, concentrating under reduced pressure to obtain crystal without water, loading into sausage casing, soaking in pure water for 2 days, dissolving, and decolorizing with S-8 macroporous resin;
(4) b3, adding 3 times of anhydrous ethanol, continuously stirring overnight, centrifuging, and drying the obtained precipitate; adding 1.5L deionized water into the dried precipitate to dissolve the precipitate to obtain ilex latifolia polysaccharide extractive solution;
(5) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 100mLFeSO4·7H2Slowly dripping O solution into 500mL ilex latifolia polysaccharide extract, stirring, and FeSO4Continuously stirring the solution for 30min after the dropwise addition is finished until the reaction is complete;
(6) and (4) filtering the reaction liquid obtained after the step S1, washing the rest solid for multiple times by using ethanol, transferring the solid into a vacuum drying oven at 70 ℃ for drying overnight, taking out the solid after the drying is finished, and smashing and grinding the solid to obtain the product of the nano iron particles.
Example 6
A method for green synthesis of nano-iron by using ilex latifolia comprises the following specific steps:
(1) weighing 40g of dried and ground ilex latifolia powder, and respectively leaching with 350mL of 80% ethanol for 2 times, each time for 1 h;
(2) heating the residue in water bath at 80 deg.C, and extracting with deionized water for 2.5 hr for 4 times;
(3) mixing the extractive solutions, transferring into rotary evaporator, concentrating under reduced pressure to obtain crystal without water, loading into sausage casing, soaking in pure water for 3 days, dissolving, and decolorizing with S-8 macroporous resin;
(4) b3, adding 3 times of anhydrous ethanol, continuously stirring overnight, centrifuging, and drying the obtained precipitate; adding 1L deionized water into the dried precipitate to dissolve the precipitate to obtain ilex latifolia polysaccharide extractive solution;
(5) preparing 0.10mol/L FeSO4·7H2O solution, under the protection of nitrogen, 200mLFeSO4·7H2Slowly dripping O solution into 1L of ilex latifolia polysaccharide extractive solution, stirring, and adding FeSO4Continuously stirring the solution for 30min after the dropwise addition is finished until the reaction is complete;
(6) filtering the reaction solution obtained in step S1, washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at 60 deg.C for drying overnight, taking out the solid after drying, mashing and grinding to obtain nanometer iron particles
Among them, the nano-iron particles prepared according to examples 1 to 6 of the present invention were R-Fe NPs.
Comparative example 1
Weighing 60g of dry and ground folium Ilicis Purpureae, placing in a reaction container, weighing 1L of deionized water, adding into the container, heating at 80 deg.C for 1 hr, filtering to obtain filtrate, and preparing 200mL of 0.10mol/L FeSO4·7H2O solution under the protection of nitrogenSlowly dripping into 1L of ilex latifolia extractive solution, stirring, and adding FeSO4Stirring for 20min after the solution is dropwise added, filtering the reaction solution, washing the remaining solid with ethanol, transferring to a vacuum drying oven at 60 ℃ for drying overnight, taking out after the drying is finished, and appropriately mashing and grinding, wherein the obtained product is nano iron particles (H-Fe NPs).
Comparative example 2
The ethyl acetate-extracted organic phase remaining after the method of examples 1 to 3 was taken as a reducing agent, and 200mL of 0.10mol/L FeSO was prepared4·7H2O solution, under nitrogen, was added slowly dropwise to the 1L ethyl acetate extracted organic phase, with constant stirring, FeSO4Stirring for 20min after the solution is dropwise added, filtering the reaction solution, washing the remaining solid with ethanol, transferring to a vacuum drying oven at 60 ℃ for drying overnight, taking out after the drying is finished, and appropriately mashing and grinding, wherein the obtained product is the nano iron particles (Ea-Fe NPs).
Performance testing
1. The principle of green synthesis of nano-iron by using ilex latifolia is shown in figure 1, wherein polysaccharide extract in ilex latifolia is reacted with ferrous ions to obtain black solid powder which is nano-iron particles, mainly Fe2+Is electrostatically attracted by negatively charged oxygen atoms (e.g., hydroxyl, etheroxy, etc.) on the polysaccharide, followed by Fe2+Reducing with aldehyde group on polysaccharide to generate Fe0The nuclei, and the aldehyde groups are oxidized to carboxyl groups, which is continuously carried out around the polysaccharide molecule, Fe0The crystal nucleus slowly grows into nano iron particles.
2. The morphology of H-Fe NPs is characterized and analyzed by TEM and HRTEM, as shown in figure 2(a) (b), the green synthesized nano-iron is observed to be mainly spherical and connected into a network chain distribution by organic matter, the nano-iron is coated with a thin shell, the interior is black nano-iron material with the particle size of about 110nm, figure 2(c) is observed by HRTEM on the lattice morphology of the surface layer of the nano-iron particle, the nano-iron has visible lattice fringe spacing of 0.253nm and 0.262nm, and the corresponding lattice spacingThe (311) lattice plane and the (109) lattice plane correspond to inverse spinel Fe3O4 and gamma-Fe 2O3 iron oxide series substances, respectively, so that when the green synthesis of the nano-iron is carried out, part of oxygen-containing groups and Fe in the solution2+Fast reaction to produce iron oxide Fe3O4And Fe2O3And a unique shell-core structure is formed, and the structure plays a unique role in the transmission of electrons in chemical reaction, and after the green synthesized nano iron is placed at room temperature for 48 hours, macroscopic agglomeration does not occur, so that the shell-core structure on the surface of the particle enables the particle to be better dispersed in a solution through electrostatic repulsion and steric hindrance.
3. The invention carries out qualitative analysis on the main biological components in the ilex latifolia extract before and after the reaction respectively, and carries out quantitative analysis on the content of the main biological components, the result is shown in table 1, alkaloid, polyphenol and flavonoid substances mainly exist in an organic phase extracted by ethyl acetate, and a small amount of flavone, polyphenol and a large amount of carbohydrate mainly exist in a residual water phase after the extraction.
TABLE 1 reaction phenomena of biological Components
| Extracting phase | Alkaloid | Flavone | Phenols | Sugar and glycoside |
| Ether (A) | Is composed of (purple) | Is (peach red) | Is composed of (purple) | - |
| Ethyl acetate | Is composed of (purple) | Is (peach red) | Is composed of (purple) | Microscale (brick red) |
| Water (W) | - | Micro (peach red) | Micro (purple) | Is (brick red) |
4. And (3) testing the reactivity:
preparing a methylene blue solution with the concentration of 50.0mg/L, adding the nano-iron particles prepared by the methods of the invention embodiment 1, the comparison embodiment 1 and the comparison embodiment 2 into the methylene blue solution, reacting the nano-iron particles with the methylene blue solution at the reaction temperature of 25 ℃, centrifuging a sample after the reaction is finished, then performing suction filtration on the solution, measuring the absorbance of the solution after the suction filtration under the wavelength of 665nm by using an ultraviolet spectrophotometer, and calculating the removal rate, wherein the specific results are shown in figure 3, and when the reaction time is 30min, the removal rates of Ea-Fe NPs, H-Fe NPs and R-Fe NPs on the methylene blue are respectively 41.4%, 46.6% and 63.2%; when the reaction time is 60min, the removal effect is increased slowly, and the removal rates are respectively 50.8%, 52.9% and 69.6%; and when the reaction proceeded for 300min, the removal rates of methylene blue were 70.7%, 88.9% and 92.1%, respectively. According to the analysis, the removal rate of the R-Fe NPs of the nano-iron particles prepared by the method to the methylene blue is larger than the degradation rate of the H-Fe NPs to the methylene blue, and the removal rate of the H-Fe NPs to the methylene blue is larger than the degradation rate of the Ea-Fe NPs to the methylene blue; wherein Ea-Fe NPs mainly comprise polyphenol and flavonoid substances in ilex latifolia and Fe2+The R-Fe NPs mainly comprise polysaccharides and Fe in ilex latifolia2+The nano-iron formed by the reaction, H-Fe NPs are the nano-iron formed by the reaction of various substances in the extracting solution and Fe2+, and visible polysaccharide substances and Fe2+The activity of the nano-iron generated by the reaction is higher, mainly because the polysaccharide substance is a macromolecule, the polysaccharide substance has larger molecular weight, more complex spatial structure and more effective electron transfer mode, so that the nano-iron synthesized by the polysaccharide substance has the highest reaction activity.
5. Collecting coal imported from a Hongka harbor area, crushing, dividing and the like the coal sample, passing through a screen with the aperture of 3mm, and dividing and sampling the sample by a bipartition device. The selected leaching column is a glass tube with the diameter of 600cm, and a sintered quartz sand plug is arranged at the lower end of the leaching column for sealing. And (3) preparing dilute nitric acid with the concentration of 5% to wash the glass tube and the quartz sand plug below the glass tube, pouring standard sand into the glass tube after three times of washing, paving the glass tube with the thickness of 5cm, pouring the extracted sample into the glass tube with the height of about 45cm, paving the standard sand on the uppermost layer, paying attention to that the layer is thinner, and regulating and controlling the flow rate of the sample through a Ma bottle. When leaching is carried out, simulation is carried out by combining the actual condition of local rainfall, the used liquid is distilled water, the duration of the process is 5 days, the simulated leaching condition is corresponding to the rainfall within 10 years of the local area, and the sampling frequency is 10. The concentrations of heavy metals (Pb, As, Cr and Cd) were determined according to the Water and wastewater monitoring method, and the contents of heavy metals (Pb, As, Cr and Cd) were determined by ICPMS. 2.0mg/mL of nano-iron particles prepared by the method are mixed into the standard sand at the lower layer of the leaching column, and other leaching experimental steps are planned as before.
The method comprises the steps of precisely measuring 100mL of water sample, filtering, receiving filtrate in a beaker, transferring 5mL of nitric acid into the beaker, transferring the nitric acid to an electric heating plate for heating, wherein the final volume needs to be controlled to be 10mL, so that effective digestion can be realized, transferring 5mL of nitric acid and 2mL of perchloric acid, adding the nitric acid and the perchloric acid into the beaker, continuously digesting until the final volume is about the residual l mL, and continuously repeating the operation if complete digestion cannot be realized. Finally, the obtained solution is fixed to a 25mL volumetric flask by pure water, a blank test is carried out in the whole digestion process, and the result is shown in FIG. 4, the green synthesized nano-iron has the removal effect on Pb, As, Cr and Cd metal ions, and the removal rates are 94.5%, 81.4%, 84.3% and 66.7% respectively.
6. Referring to the attached figure 5, the research on degrading phenanthrene, anthracene and pyrene in soil by using the green synthesized nano iron prepared by the invention as a catalyst for catalyzing Fenton-like reaction is shown, the contents of phenanthrene (phenanthrene), anthracene (anthrene) and Pyrene (Pyrene) in the polluted soil are respectively 328mg/kg, 246mg/kg and 407mg/kg through GC-MS analysis, during the reaction time of 24h, a batch was terminated every 4h, and the reactant content was measured, as can be seen from FIG. 5, in actual soil, the phenanthrene, anthracene and pyrene are degraded by the Fenton-like reaction under the catalysis of green synthesized nano iron for four hours, the degradation rates are respectively 29.3 percent, 24.5 percent and 26.1 percent, the degradation rates after 24 hours respectively reach 67.4 percent, 70.2 percent and 70.4 percent, compared with the simulated soil PAHs degraded by Fenton reaction catalyzed by green synthetic nano-iron, the simulated soil PAHs degraded by the green synthetic nano-iron serving as the catalyst of the Fenton reaction has certain practical application prospect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A method for green synthesis of nano-iron by using ilex latifolia is characterized by comprising the following specific steps:
(1) extracting polysaccharide substances in the ilex latifolia to obtain a polysaccharide extracting solution;
(2) polysaccharide solution is used as a reducing agent to reduce iron salt to prepare green synthetic nano iron.
2. The method for green synthesis of nano-iron by using ilex latifolia as claimed in claim 1, wherein the method comprises the following steps: the specific steps for preparing the polysaccharide extracting solution in the step (1) are as follows:
a1, weighing 30-60 g of dry and ground ilex latifolia powder, adding 0.8-1L of distilled water, heating in a water bath at 80-90 ℃ for 1-1.5 h, and performing suction filtration for later use;
a2, separating 400-500 mL of filtrate, extracting with ethyl acetate or ether for multiple times for 2-4 min respectively, and combining aqueous phase liquid obtained after multiple ethyl acetate or ether extractions to serve as ilex latifolia polysaccharide extracting solution for later use.
3. The method for green synthesis of nano-iron by using ilex latifolia as claimed in claim 3, wherein the method comprises the following steps: and B, extracting the filtrate by using ethyl acetate or ethyl ether in the step A2 for 3 times respectively, and extracting by using 100-200 mL of ethyl acetate or ethyl ether each time.
4. The method for green synthesis of nano-iron by using ilex latifolia as claimed in claim 1, wherein the method comprises the following steps: the specific steps for preparing the polysaccharide extracting solution in the step (1) are as follows:
b1, weighing 30-60 g of dried and ground ilex latifolia powder, and leaching for at least 2 times with 250-500 mL of 80% ethanol for 1-2 hours each time;
b2, heating the residual residues in a water bath at the temperature of 80-90 ℃ after leaching, and respectively extracting with deionized water for at least 3 times, wherein each extraction needs 2-2.5 hours;
b3, combining the multiple extracting solutions, transferring the extracting solutions into a rotary evaporator, concentrating under a reduced pressure condition to enable the extracting solutions to be in a final crystallization moisture-free state, filling the concentrated solution into a sausage casing, soaking the concentrated solution into pure water for 2-3 days, dissolving the concentrated solution again, and decolorizing the concentrated solution through S-8 macroporous resin;
b4, adding 3 times of volume of absolute ethyl alcohol into the extract obtained in the step B3, continuously stirring the mixture overnight, then carrying out centrifugal treatment, and drying the obtained precipitate; adding 1-1.5L of deionized water into the dried precipitate to dissolve the precipitate to prepare ilex latifolia polysaccharide extracting solution;
5. the method for green synthesis of nano-iron by using ilex latifolia as claimed in claim 1, wherein the method comprises the following steps: the specific steps for preparing the green synthetic nano-iron in the step (2) are as follows:
s1, preparing 0.10mol/L FeSO4·7H2Adding O solution slowly dropwise into the polysaccharide extract of ilex latifolia under nitrogen protection, stirring, and adding FeSO4Continuously stirring for 20-30 min after the solution is dripped until the reaction is complete;
s2, filtering the reaction liquid obtained in the step S1, washing the rest solid with ethanol for multiple times, transferring the solid into a vacuum drying oven at the temperature of 60-70 ℃ for drying overnight, taking out the dried solid after drying, and smashing and grinding the dried solid to obtain the product of the nano iron particles.
6. The method for green synthesis of nano-iron by using ilex latifolia as claimed in claim 1, wherein the method comprises the following steps: the ilex latifolia polysaccharide extracting solution and FeSO in the step S14·7H2The volume ratio of the O solution is 5: 1.
7. The green synthesized nano-iron prepared by the method according to any one of claims 1 to 6 is applied to the remediation of water and soil environments polluted by heavy metals and polycyclic aromatic hydrocarbons.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114029502A (en) * | 2021-11-12 | 2022-02-11 | 中国科学院合肥物质科学研究院 | Method for synthesizing nano platinum by using artemisia apiacea extract and application |
| CN114749675A (en) * | 2022-02-28 | 2022-07-15 | 南开大学 | Method for green continuous synthesis of nano-iron and nano-iron composite material |
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