CN104071799B - A kind of talcum-magnetic metal nano composite material and preparation method thereof - Google Patents
A kind of talcum-magnetic metal nano composite material and preparation method thereof Download PDFInfo
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- CN104071799B CN104071799B CN201410316575.4A CN201410316575A CN104071799B CN 104071799 B CN104071799 B CN 104071799B CN 201410316575 A CN201410316575 A CN 201410316575A CN 104071799 B CN104071799 B CN 104071799B
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Abstract
The invention discloses a kind of talcum-magnetic metal nano composite material and preparation method thereof. Magnetic metal nanoparticle is positioned at talcum interlayer. Preparation process is: first by talcum separating-purifying, then mix by a certain percentage with the metallorganic of preparation; Utilize the hydrophobicity of talcum interlayer that metallorganic intercalation is entered to talcum interlayer; After high temperature thermal decomposition, obtain metal oxide microparticle in talcum interlayer original position; To after metal oxide reduction, obtain talcum-magnetic metal nano composite material. Due to restraining force and the confinement effect of talcum interlayer, synthetic talcum-magnetic metal nano composite material has Stability Analysis of Structures, uniform particle diameter, the active feature such as strong, has potential purposes in fields such as refractory wastewater, electro-magnetic wave absorption, magnetic resonance images.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of talcum-magnetic metal 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 properties of talcum, talcum is mainly used in filler, insulating materials, lubricant, agricultural chemicals absorbent, leather coating, the cosmetic of refractory material, 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 (PhysChemMinerals, 1991,17:611-616) that can not intercalation, this has limited the development of talcum in function mineral field widely. Magnetic metal 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 conductivity and the feature such as dielectric constant is large, magnetic metal nanoparticle has excellent catalytic performance and electro-magnetic wave absorption performance.
But yet there are no the report that talcum is combined with magnetic metal particulate, especially magnetic metal particulate is positioned at the report of talcum interlayer. This is to perplex researcher because ion intercalation is entered to this difficult problem of talcum interlayer always. In addition, due to restraining force and the confinement effect of talcum interlayer, magnetic metal 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-magnetic metal nano composite material and preparation method thereof is provided.
The present invention combines magnetic metal nanoparticle with talcum mineral, utilize the hydrophobicity of talcum interlayer, adopt high shear grinding legal system standby there is talcum-magnetic metal nano composite material of unique texture. Magnetic metal 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, electro-magnetic wave absorption, magnetic resonance images.
A kind of talcum-magnetic metal nano composite material, it is a kind of nano composite material being made up of talcum and magnetic metal nanoparticle, described magnetic metal nanoparticle is positioned at talcum interlayer, described magnetic metal particulate is one or more alloys in Fe, Co, Ni, Mn or Zn, and the particle diameter of magnetic metal particulate is 1～100nm.
A preparation method for described talcum-magnetic metal 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 sodium dithionite 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 centrifugal dehydration are cleaned, 60 to 150 DEG C of oven dry;
3) metallorganic 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 15～120min is 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-magnetic metal nano composite material.
Preferably, described metallorganic is one or more in the stearate of oleate, Mn, Fe, Ni, Cu, Co or Zn or the citrate 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, oxolane, chloroform, dimethyl formamide, acetone or n-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 raw material that talcum-magnetic metal nano composite material of proposition and preparation method thereof takes full advantage of talcum mineral, due to restraining force and the confinement effect of talcum interlayer, the novel nano composite obtaining has Stability Analysis of Structures, uniform particle diameter, the active feature such as strong, has potential purposes in fields such as refractory wastewater, electro-magnetic wave absorption, magnetic resonance images. Talcum-magnetic metal nano composite material that the present invention proposes and preparation method thereof, technological process is simple, material structure novelty, potential use is extensive, has very strong using value.
Detailed description of the invention
The present invention proposes a kind of talcum-magnetic metal nano composite material and preparation method thereof. Detailed description of the invention 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, hydroxide, processes these Impurity removals that exist in talcum by hydrochloric acid and sodium dithionite. Subsequently mineral are filtered or centrifugal 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 metallorganic mixture. Due to talcum interlayer meeting hydrophobicity, therefore having nonpolar metallorganic could enter talcum interlayer by intercalation. A certain amount of divalent metal organic matter or metallorganic mixture (metallorganic of selecting comprises oleate, stearate or the citrate of Mn, Fe, Ni, Cu, Co or Zn metal) are joined and common are machine solvent as in ethanol, oxolane, chloroform, dimethyl formamide, acetone or n-hexane, and metal species and ratio regulate according to actual needs.
The 3rd step of preparation is that metallorganic intercalation is entered to talcum interlayer, and its original position is synthesized to magnetic metal nanoparticle. Talcum is joined in the metallorganic 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, metallorganic is decomposed into metal oxide (reaction 1) in nanotube inside; Then switch atmosphere, reduce 15～120min 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-magnetic metal nano composite material. The reaction equation following (taking iron oleate as example) of this process:
Fe-Oleate→Fe2O3（1）
Fe2O3+3H2=2Fe+3H2O（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 sodium dithionite 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 centrifugal 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 120min is 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 sodium dithionite 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 centrifugal 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 15min is 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 sodium dithionite 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 centrifugal dehydration are cleaned, 70 DEG C of oven dry;
3) ferric stearate of 0.1 mole is joined in 0.2 liter of oxolane 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 100min is 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 sodium dithionite 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 centrifugal 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 90min is 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 sodium dithionite 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 centrifugal dehydration are cleaned, 90 DEG C of oven dry;
3) copper 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 75min is 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 sodium dithionite 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 centrifugal 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 n-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 60min is 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 sodium dithionite 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 centrifugal 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 45min is 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 (4)
1. talcum-magnetic metal nano composite material, it is characterized in that, it comprises talcum and magnetic metal nanoparticle, described magnetic metal nanoparticle is positioned at talcum interlayer, described magnetic metal nanoparticle is the alloy of one or more element compositions in Fe, Co, Ni, Mn or Zn, and the particle diameter of magnetic metal nanoparticle is 1～100nm.
2. a preparation method for talcum-magnetic metal 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 sodium dithionite 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 centrifugal dehydration are cleaned, 60 to 150 DEG C of oven dry;
3) the magnetic metal organic matter 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 15～120min is 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-magnetic metal nano composite material;
Described magnetic metal organic matter is one or more in the stearate of oleate, Mn, Fe, Ni, Cu, Co or Zn or the citrate of Mn, Fe, Ni, Cu, Co or Zn of business or homemade Mn, Fe, Ni, Cu, Co or Zn.
3. preparation method according to claim 2, is characterized in that, described organic solvent is one or more in ethanol, oxolane, chloroform, dimethyl formamide, acetone or n-hexane.
4. 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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| 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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