CN104071799A - Talc-magnetic metal nano composite material and preparation method thereof - Google Patents
Talc-magnetic metal nano composite material and preparation method thereof Download PDFInfo
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- CN104071799A CN104071799A CN201410316575.4A CN201410316575A CN104071799A CN 104071799 A CN104071799 A CN 104071799A CN 201410316575 A CN201410316575 A CN 201410316575A CN 104071799 A CN104071799 A CN 104071799A
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- talcum
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Abstract
The invention discloses a talc-magnetic metal nano composite material and a preparation method thereof. Magnetic metal nano particles are positioned between talc layers. The preparation method comprises the steps of separating and purifying talc, and then mixing the talc and a prepared metal organic matter according to a certain proportion; intercalating the metal organic matter into the talc layers by using the hydrophobic property between the talc layers; performing high temperature cracking to obtain metal oxide particles between the talc layers in situ; reducing the metal oxide to obtain the talc-magnetic metal nano composite material. Due to the constraining force and confinement effect between the talc layers, the synthesized talc-magnetic metal nano composite material has the characteristics of stable structure, uniform particle diameter, strong activity and the like, so that the composite material has a potential application in the fields of non-degradable wastewater treatment, electromagnetic wave absorption, magnetic resonance imaging and the like.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of talcum-magneticmetal nano composite material and preparation method thereof.
Background technology
Talcum is a kind of common layer silicate mineral, has very soft and satiny feel, and this hardness of rubbing is only 1.Due to the physicochemical property of talcum, talcum is mainly used in filler, insulating material, lubricant, agricultural chemicals absorption agent, leather coating, the cosmetic of refractory materials, papermaking, rubber and carves the fields such as materials at present.But different from general layer silicate mineral, talcum is acknowledged as a kind of mineral (Phys Chem Minerals, 1991,17:611-616) that can not intercalation, this has limited the development of talcum in function mineral field widely.Magneticmetal nanoparticle comprises Fe, Ni, Co, Mn, Zn and alloy thereof etc., has broad application prospects.Because its density is little, Curie temperature is high, Heat stability is good, magnetic permeability and the feature such as specific inductivity is large, magneticmetal nanoparticle has excellent catalytic performance and absorption of electromagnetic wave performance.
But yet there are no the report that talcum is combined with magneticmetal particulate, especially magneticmetal particulate is positioned at the report of talcum interlayer.This is to perplex researchist because ion intercalation is entered to this difficult problem of talcum interlayer always.In addition, due to restraint force and the confinement effect of talcum interlayer, magneticmetal nanoparticle is inserted to talcum interlayer and will greatly strengthen its activity, and reduce its particle diameter and change its patterned features, therefore expect and will obtain having the nano composite material of excellent properties.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of talcum-magneticmetal nano composite material and preparation method thereof is provided.
The present invention combines magneticmetal nanoparticle with talcum mineral, utilize the hydrophobicity of talcum interlayer, adopt high shear grinding legal system standby there is talcum-magneticmetal nano composite material of unique texture.Magneticmetal nanoparticle is positioned at talcum interlayer.This novel nano composite material has the feature such as Stability Analysis of Structures, uniform particle diameter, has potential purposes in fields such as refractory wastewater, absorption of electromagnetic wave, magnetic resonance images.
A kind of talcum-magneticmetal nano composite material, it is a kind of nano composite material being made up of talcum and magneticmetal nanoparticle, described magneticmetal nanoparticle is positioned at talcum interlayer, described magneticmetal particulate is one or more alloys in Fe, Co, Ni, Mn or Zn, and the particle diameter of magneticmetal particulate is 1～100 nm.
A preparation method for described talcum-magneticmetal nano composite material, step is as follows:
1) through the talcum of separating-purifying, add 5 to 10 times of weight, the hydrochloric acid of concentration 3% to 10%, then add the V-Brite B that is equivalent to talcum weight 0.5% to 2%, and stir and make suspension ore pulp, at room temperature react 6～24 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 60 to 150 DEG C of oven dry;
3) metallorganics of 0.05～0.5 mole is joined in 0.1～1 liter of organic solvent to mixing and stirring; Add 100 grams of steps 2) product of gained grinds after mixing and stirring 0.5 to 5 hour in high shear grinding machine;
4) 60～150 DEG C of oven dry of products therefrom are placed in stove, and 15～120 min are reduced in 450～900 DEG C of calcinings 0.5～3 hour subsequently in nitrogen/hydrogen mixed gas atmosphere of 450～800 DEG C; Cooling rear taking-up, obtains talcum-magneticmetal nano composite material.
Preferably, described metallorganics is one or more in the stearate of oleate, Mn, Fe, Ni, Cu, Co or Zn or the Citrate trianion of Mn, Fe, Ni, Cu, Co or Zn of business or homemade Mn, Fe, Ni, Cu, Co or Zn.
Preferably, described organic solvent is one or more in ethanol, tetrahydrofuran (THF), chloroform, dimethyl formamide, acetone or normal hexane.
Preferably, described high shear grinding machine is the one in ball mill, roller mill, rod mill, ball mill.
Beneficial effect of the present invention: it is starting material that talcum-magneticmetal nano composite material of proposition and preparation method thereof takes full advantage of talcum mineral, due to restraint force and the confinement effect of talcum interlayer, the novel nano matrix material obtaining has Stability Analysis of Structures, uniform particle diameter, the active feature such as strong, has potential purposes in fields such as refractory wastewater, absorption of electromagnetic wave, magnetic resonance images.Talcum-magneticmetal nano composite material that the present invention proposes and preparation method thereof, technical process is simple, material structure novelty, potential use is extensive, has very strong using value.
Embodiment
The present invention proposes a kind of talcum-magneticmetal nano composite material and preparation method thereof.Embodiment comprises the following steps:
The first step of preparation is that talcum removal of impurities is purified.Naturally occurring talcum contains the impurity such as quartz, iron and manganese oxides, oxyhydroxide, processes these Impurity removals that exist in talcum by hydrochloric acid and V-Brite B.Subsequently mineral are filtered or centrifuge dehydration, after the thorough cleaning, drying of deionized water, obtain the talcum mineral that purity is higher.
The second step of preparation is to prepare metallorganics mixture.Due to talcum interlayer meeting hydrophobicity, therefore having nonpolar metallorganics could enter talcum interlayer by intercalation.A certain amount of divalent metal organism or metallorganics mixture (metallorganics of selecting comprises oleate, stearate or the Citrate trianion of Mn, Fe, Ni, Cu, Co or Zn metal) are joined and common are machine solvent as in ethanol, tetrahydrofuran (THF), chloroform, dimethyl formamide, acetone or normal hexane, and metal species and ratio regulate according to actual needs.
The 3rd step of preparation is that metallorganics intercalation is entered to talcum interlayer, and its original position is synthesized to magneticmetal nanoparticle.Talcum is joined in the metallorganics mixture that step 2 obtains, and after mixing and stirring, sample grinds 0.5 to 5 hour in high shear grinding machine, makes intercalation complete as far as possible.Product is dried and is placed in stove, calcine 0.5～3 hour for 450～900 DEG C, metallorganics is decomposed into metal oxide (reaction 1) in nanotube inside; Then switch atmosphere, reduce 15～120 min in nitrogen/hydrogen mixed gas atmosphere of 450～800 DEG C, metal oxide is reduced to metal simple-substance nanoparticle (reaction 2).Cooling rear taking-up, obtains talcum-magneticmetal nano composite material.The reaction equation following (taking iron oleate as example) of this process:
Fe-Oleate → Fe
2O
3 （1）
Fe
2O
3 + 3H
2 = 2Fe + 3H
2O （2）
Further illustrate the present invention below in conjunction with embodiment.
embodiment 1
1) through the talcum of separating-purifying, add the hydrochloric acid of 5 weight concentrations 10%, then add the V-Brite B that is equivalent to talcum weight 0.5%, stir and make suspension ore pulp, at room temperature react 24 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 60 DEG C of oven dry;
3) manganese oleate of 0.05 mole is joined in 0.1 liter of ethanol to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 0.5 hour after mixing and stirring in high shear grinding machine;
4) 150 DEG C of oven dry of products therefrom are placed in stove, and 120 min are reduced in 450 DEG C of calcinings 3 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 450 DEG C; Cooling rear taking-up, obtains talcum-simple substance manganese nano composite material.
embodiment 2
1) through the talcum of separating-purifying, add the hydrochloric acid of 10 times of weight concentrations 3%, then add the V-Brite B that is equivalent to talcum weight 2%, stir and make suspension ore pulp, at room temperature react 6 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 150 DEG C of oven dry;
3) the oleic acid nickel of 0.5 mole is joined in 1 liter of acetone to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 5 hours after mixing and stirring in high shear grinding machine;
4) 60 DEG C of oven dry of products therefrom are placed in stove, and 15 min are reduced in 900 DEG C of calcinings 0.5 hour subsequently in nitrogen/hydrogen mixed gas atmosphere of 800 DEG C; Cooling rear taking-up, obtains talcum-elemental nickel nano composite material.
embodiment 3
1) through the talcum of separating-purifying, add 6 times of weight, the hydrochloric acid of concentration 9%, then add the V-Brite B that is equivalent to talcum weight 1.5%, and stir and make suspension ore pulp, at room temperature react 18 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 70 DEG C of oven dry;
3) iron stearate of 0.1 mole is joined in 0.2 liter of tetrahydrofuran (THF) to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 1 hour after mixing and stirring in high shear grinding machine;
4) 70 DEG C of oven dry of products therefrom are placed in stove, and 100 min are reduced in 500 DEG C of calcinings 2.5 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 500 DEG C; Cooling rear taking-up, obtains talcum-fe nano composite material.
embodiment 4
1) through the talcum of separating-purifying, add 8 times of weight, the hydrochloric acid of concentration 5%, then add the V-Brite B that is equivalent to talcum weight 1%, and stir and make suspension ore pulp, at room temperature react 12 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 80 DEG C of oven dry;
3) zinc citrate of 0.2 mole is joined in 0.4 liter of chloroform to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 1.5 hours after mixing and stirring in high shear grinding machine;
4) 80 DEG C of oven dry of products therefrom are placed in stove, and 90 min are reduced in 600 DEG C of calcinings 2 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 550 DEG C; Cooling rear taking-up, obtains talcum-simple substance zinc nano composite material.
embodiment 5
1) through the talcum of separating-purifying, add 7 times of weight, the hydrochloric acid of concentration 6%, then add the V-Brite B that is equivalent to talcum weight 1.2%, and stir and make suspension ore pulp, at room temperature react 15 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 90 DEG C of oven dry;
3) cupric oleate of 0.3 mole is joined in 0.6 liter of dimethyl formamide to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 2 hours after mixing and stirring in high shear grinding machine;
4) 90 DEG C of oven dry of products therefrom are placed in stove, and 75 min are reduced in 650 DEG C of calcinings 2 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 600 DEG C; Cooling rear taking-up, obtains talcum-elemental copper nano composite material.
embodiment 6
1) through the talcum of separating-purifying, add 6 times of weight, the hydrochloric acid of concentration 7%, then add the V-Brite B that is equivalent to talcum weight 0.8%, and stir and make suspension ore pulp, at room temperature react 8 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 120 DEG C of oven dry;
3) the iron oleate mixture of the cobalt oleate of each 0.2 mole is joined in 0.5 liter of normal hexane to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 2.5 hours after mixing and stirring in high shear grinding machine;
4) 100 DEG C of oven dry of products therefrom are placed in stove, and 60 min are reduced in 700 DEG C of calcinings 1.5 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 650 DEG C; Cooling rear taking-up, obtains talcum-CoFe nano composite material.
embodiment 7
1) through the talcum of separating-purifying, add 5 times of weight, the hydrochloric acid of concentration 9%, then add the V-Brite B that is equivalent to talcum weight 0.6%, and stir and make suspension ore pulp, at room temperature react 20 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 140 DEG C of oven dry;
3) iron oleate of 0.25 mole is joined in 0.25 liter of ethanol to mixing and stirring; Add 100 grams of steps 2) product of gained grinds 3 hours after mixing and stirring in high shear grinding machine;
4) 110 DEG C of oven dry of products therefrom are placed in stove, and 45 min are reduced in 750 DEG C of calcinings 1.5 hours subsequently in nitrogen/hydrogen mixed gas atmosphere of 700 DEG C; Cooling rear taking-up, obtains talcum-fe nano composite material.
Claims (5)
1. talcum-magneticmetal nano composite material, it is characterized in that, it comprises talcum and magneticmetal nanoparticle, described magneticmetal nanoparticle is positioned at talcum interlayer, described magneticmetal particulate is one or more alloys in Fe, Co, Ni, Mn or Zn, and the particle diameter of magneticmetal particulate is 1～100 nm.
2. a preparation method for talcum-magneticmetal nano composite material, is characterized in that, step is as follows:
1) through the talcum of separating-purifying, add 5 to 10 times of weight, the hydrochloric acid of concentration 3% to 10%, then add the V-Brite B that is equivalent to talcum weight 0.5% to 2%, and stir and make suspension ore pulp, at room temperature react 6～24 hours, constantly stir during this time;
2) after products therefrom filtration or centrifuge dehydration are cleaned, 60 to 150 DEG C of oven dry;
3) metallorganics of 0.05～0.5 mole is joined in 0.1～1 liter of organic solvent to mixing and stirring; Add 100 grams of steps 2) product of gained grinds after mixing and stirring 0.5 to 5 hour in high shear grinding machine;
4) 60～150 DEG C of oven dry of products therefrom are placed in stove, and 15～120 min are reduced in 450～900 DEG C of calcinings 0.5～3 hour subsequently in nitrogen/hydrogen mixed gas atmosphere of 450～800 DEG C; Cooling rear taking-up, obtains talcum-magneticmetal nano composite material.
3. preparation method according to claim 2, it is characterized in that, described metallorganics is one or more in the stearate of oleate, Mn, Fe, Ni, Cu, Co or Zn or the Citrate trianion of Mn, Fe, Ni, Cu, Co or Zn of business or homemade Mn, Fe, Ni, Cu, Co or Zn.
4. preparation method according to claim 2, is characterized in that, described organic solvent is one or more in ethanol, tetrahydrofuran (THF), chloroform, dimethyl formamide, acetone or normal hexane.
5. preparation method according to claim 2, is characterized in that described high shear grinding machine is the one in ball mill, roller mill, rod mill, ball mill.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108806907A (en) * | 2018-05-31 | 2018-11-13 | 浙江大学 | The new application of manganese nodule and the preparation method of stratiform intercalated magnetic metallic composite |
| CN112592487A (en) * | 2020-12-11 | 2021-04-02 | 成都理工大学 | Adenine and citric acid with Zn2+Constructed MOFs material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164131A1 (en) * | 2011-06-03 | 2012-12-06 | Nanobiomatters Research & Development, S. L. | Nanocomposite materials based on metal oxides having multi-functional properties |
| CN103408288A (en) * | 2013-08-13 | 2013-11-27 | 浙江大学 | Tubular clay mineral-ferrite nanocomposite and preparation method thereof |
| CN103482636A (en) * | 2013-10-12 | 2014-01-01 | 冕宁锡成滑石矿业有限责任公司 | Method for removing calcium oxide for whitening by using low-whiteness talcum powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164131A1 (en) * | 2011-06-03 | 2012-12-06 | Nanobiomatters Research & Development, S. L. | Nanocomposite materials based on metal oxides having multi-functional properties |
| CN103408288A (en) * | 2013-08-13 | 2013-11-27 | 浙江大学 | Tubular clay mineral-ferrite nanocomposite and preparation method thereof |
| CN103482636A (en) * | 2013-10-12 | 2014-01-01 | 冕宁锡成滑石矿业有限责任公司 | Method for removing calcium oxide for whitening by using low-whiteness talcum powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108806907A (en) * | 2018-05-31 | 2018-11-13 | 浙江大学 | The new application of manganese nodule and the preparation method of stratiform intercalated magnetic metallic composite |
| CN112592487A (en) * | 2020-12-11 | 2021-04-02 | 成都理工大学 | Adenine and citric acid with Zn2+Constructed MOFs material and preparation method thereof |
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