CN105731552B - Talc-titanic acid nickel nanocomposite and preparing method thereof - Google Patents
Talc-titanic acid nickel nanocomposite and preparing method thereof Download PDFInfo
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- CN105731552B CN105731552B CN201610068114.9A CN201610068114A CN105731552B CN 105731552 B CN105731552 B CN 105731552B CN 201610068114 A CN201610068114 A CN 201610068114A CN 105731552 B CN105731552 B CN 105731552B
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- nickel
- talcum
- talc
- titanate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a talc-titanic acid nickel nanocomposite and a preparing method thereof.Titanic acid nickel nanoparticles are located between talc layers.The preparing method comprises the steps that firstly, inorganic acid and a reducing agent are used for activating and purifying layered mineral; secondly, after acid activation, dewatering and drying are conducted; thirdly, hydrophobic titanate and nickel salt are mixed with talc, and the mixture is inserted into the talc layers through high shearing and grinding; fourthly, after pyrolysis, the titanic acid nickel nanoparticles are synthesized between the talc layers in situ, and the talc-titanic acid nickel nanocomposite is obtained.The layering constraining force of the talc on the titanic acid nickel nanoparticles effectively restrains agglomeration of the nanoparticles and enables the nanoparticles to have multiple unique physicochemical properties.Thus, prepared products have potential application in the field of electromagnetic wave adsorption.
Description
Technical field
The present invention relates to composite and preparation method thereof, more particularly to a kind of talcum-nickel titanate nano composite material and
Its preparation method.
Background technology
Absorbing material is that the absorbent with absorbent properties is scattered in the middle of binding resin and rubber.Currently, many states
Family is removed to outside the research of binding resin and the matching of material and design all studying various high performance absorbing materials,
High performance absorbing material is manufactured, core seeks to manufacture loss absorbability by force and can obtain the thunder of larger interface impedance
Up to wave absorbent, therefore, to the emphasis of the research always absorbing material research of absorbent.In numerous absorbents, at present most
It is valued mainly to have：Ferrite series absorbent, metal fine powder absorbent, point crystalline substance metallic fiber range of absorbent agent；Chirality is inhaled
Wave material；Resistant to elevated temperatures ceramic absorbing material；Conduction high polymer etc..Nickel titanate has similar structure with iron system absorbent,
With absorbing property, but its research is less, therefore, nickel ferrite based magnetic loaded is applied into absorbing material will greatly improve its range of application.
Talcum is a kind of common layer silicate mineral, refractory material, papermaking, rubber is mainly used at present and is filled out
The fields such as material, insulating materials, leather coating, cosmetic.However, from unlike general layer silicate mineral, talcum one
As be considered it is a kind of can not intercalation mineral, this greatly limits talcum function mineral field development.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of talcum-nickel titanate nano composite material and its
Preparation method.
The present invention innovatively utilizes the hydrophobicity of talcum interlayer, using titanate esters and nickel salt, so as to be prepared for having solely
The talcum of special structure-nickel titanate nano composite material.Metatitanic acid nickel nanocrystals are located at talcum interlayer, are closely tied with clay mineral
Close.Because the restraining force of talcum interlayer and confinement are acted on, this new structure has uniform particle diameter, Stability Analysis of Structures, the process can
The advantages of control.The nano composite material has potential purposes in fields such as electro-magnetic wave absorption, magnetic resonance images.
A kind of talcum-nickel titanate nano composite material, nanoparticle is inserted between the crystalline texture layer of lamellar mineral talc
A kind of composite that the nickel titanate of level is formed, the nickel titanate of described nanometer grade is entered by titanate esters and nickel salt intercalation to be slided
Between rock layers, and fabricated in situ is obtained.
A kind of preparation method of talcum-nickel titanate nano composite material, step is as follows：
1) talcum of separated purification, plus 5 to 10 times of weight, the hydrochloric acid of mass concentration 3% to 10%, add equivalent to
The sodium dithionite of talcum weight 0.5% to 2%, stirs and is made suspension ore pulp, reacts 6~24 hours at room temperature,
Period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 to 150 DEG C of drying；
3) in step 2）Product in add the nickel salt of 0.05~0.5 mole of titanate esters with 0.05~0.5 mole to rub
You are than being 1:1 is added in 0.1~2 liter of organic solvent, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
Be placed in stove after the drying of 60~150 DEG C of product, 450~900 DEG C are calcined 0.5~3 hour, are taken out after cooling, obtain final product talcum-
Nickel titanate nano composite material.
Described titanate esters are butyl titanate, isopropyl titanate, monoalkoxy unrighted acid titanate esters, isopropyl
One or more in three stearic acid acyloxy titanate esters.
Described nickel salt is one or more of nickel nitrate, nickel acetate, nickel chloride, nickel sulfate.
Described organic solvent is the one kind in ethanol, tetrahydrofuran, chloroform, dimethylformamide, acetone or n-hexane
Or it is several.
Described high shear grinding machine is the one kind in ball mill, roller mill, rod mill, ball mill.
Beneficial effects of the present invention：Talcum proposed by the present invention-nickel titanate nano composite material and preparation method thereof is fully
Natural talcum mineral be make use of for raw material, in the composite for obtaining, metatitanic acid nickel nanocrystals are located at interlayer, solve cunning
The problem of intercalation is difficult between rock layers；Confinement effect due to talcum interlayer to metatitanic acid nickel particle, the composite for obtaining has to be permitted
Many unique physicochemical properties, have potential purposes in fields such as electro-magnetic wave absorption, magnetic resonances.Cunning proposed by the present invention
Stone-nickel titanate nano composite material and preparation method thereof, technological process is simple, and material structure is novel, and potential use extensively, has
Very strong application value.Natural talcum yield is big, low cost, and the present invention is that the research of talcum and large-scale application are opened
Road.
Specific embodiment
The present invention proposes a kind of talcum-nickel titanate nano composite material and preparation method thereof, and specific embodiment includes
Following steps：The first step of preparation is by talcum removal of impurities purification.Naturally occurring talcum contains quartz, iron and manganese oxides, hydrogen-oxygen
The impurity such as compound, are processed these Impurity removals present in talcum by hydrochloric acid and sodium dithionite.Then by mineral mistake
Filter or centrifugal dehydration, purity talcum mineral higher are obtained after the drying of deionized water thoroughly cleaning.
The second step of preparation is that titanate esters and nickel salt intercalation are entered into talcum interlayer, and by its fabricated in situ for nickel titanate is received
Rice particulate.Talcum is added in mixture, because talcum interlayer is hydrophobicity, titanate esters and nickel salt presoma will be preferentially entered
Talcum interlayer.Sample grinds 0.5 to 5 hour in high shear grinding machine after mixing and stirring so that intercalation is as far as possible
Completely.Then product is dried after be placed in stove, 450~900 DEG C calcine 0.5~3 hour, after cooling take out, obtain final product talcum-
Nickel titanate nano composite material.
The present invention is further illustrated with reference to embodiment.
Embodiment 1
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.5 mole of nickel acetate of the butyl titanate with 0.5 mole after be added to
In 0.1 liter of ethanol, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 2
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.3 mole of nickel acetate of the butyl titanate with 0.3 mole after be added to
In 0.1 liter of acetone, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 3
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.3 mole of nickel nitrate of the isopropyl titanate with 0.3 mole after be added to
In 0.2 liter of n-hexane, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 4
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.5 mole of nickel nitrate of the isopropyl titanate with 0.5 mole after be added to
In 0.2 liter of ethanol, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 5
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.5 mole alkoxy unrighted acid titanate esters and 0.5 mole of nitre
It is added to after sour nickel in 0.1 liter of n-hexane, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 6
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.1 mole of nickel acetate of the isopropyl titanate with 0.1 mole after be added to
In 0.5 liter of acetone, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 7
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.4 mole of isopropyl three stearic acid acyloxy titanate esters with 0.4 mole
Nickel chloride is added in 0.5 liter of ethanol, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Embodiment 8
1) talcum of separated purification, plus 5 weight 10%（Mass concentration）Hydrochloric acid, add equivalent to talcum weight
0.5% sodium dithionite, stirs and is made suspension ore pulp, reacts 24 hours at room temperature, and period is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 DEG C of drying；
3) in step 2）Product in add 0.05 mole of nickel acetate of the butyl titanate with 0.05 mole after be added to
In 0.1 liter of tetrahydrofuran, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Institute
It is placed in stove after obtaining 60~150 DEG C of drying of product, 500 DEG C are calcined 3 hours, are taken out after cooling, obtains final product talcum-nickel titanate nanometer
Composite.
Claims (5)
1. the preparation method of a kind of talcum-nickel titanate nano composite material, it is characterised in that step is as follows：
1) talcum of separated purification, plus 5 to 10 times of weight, and the hydrochloric acid of mass concentration 3% to 10% is added equivalent to talcum
The sodium dithionite of weight 0.5% to 2%, stirs and is made suspension ore pulp, reacts 6~24 hours at room temperature, period
It is stirred continuously；
2) after products therefrom filtering or centrifugal dehydration are cleaned, 60 to 150 DEG C of drying；
3) in step 2）Product in add 0.05~0.5 mole of titanate esters with 0.05~0.5 mole of nickel salt with mol ratio
It is 1:1 is added in 0.1~2 liter of organic solvent, mixing and stirring；
4) by 100 grams of steps 3）Product mixing and stirring after in high shear grinding machine grind 0.5 to 5 hour；Gained is produced
It is placed in stove after 60~150 DEG C of drying of thing, 450~900 DEG C are calcined 0.5~3 hour, are taken out after cooling, obtain final product talcum-metatitanic acid
Nickel nano composite material.
2. preparation method according to claim 1, it is characterised in that described titanate esters are different butyl titanate, metatitanic acid
One or more in propyl ester, monoalkoxy unrighted acid titanate esters, the stearic acid acyloxy titanate esters of isopropyl three.
3. preparation method according to claim 1, it is characterised in that described nickel salt is nickel nitrate, nickel acetate, chlorination
One or more of nickel, nickel sulfate.
4. preparation method according to claim 1, it is characterised in that described organic solvent is ethanol, tetrahydrofuran, chlorine
One or more in imitative, dimethylformamide, acetone or n-hexane.
5. preparation method according to claim 1, it is characterised in that described high shear grinding machine is that ball mill, roller grind
One kind in machine, rod mill, ball mill.
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| CN201610068114.9A CN105731552B (en) | 2016-02-01 | 2016-02-01 | Talc-titanic acid nickel nanocomposite and preparing method thereof |
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| CN201610068114.9A CN105731552B (en) | 2016-02-01 | 2016-02-01 | Talc-titanic acid nickel nanocomposite and preparing method thereof |
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| CN105731552B true CN105731552B (en) | 2017-05-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2757656C1 (en) * | 2021-02-19 | 2021-10-19 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for obtaining a coating from single-phase nickel titanate on a corundum substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101880067B (en) * | 2010-07-15 | 2011-12-28 | 陕西科技大学 | Preparation method of bar-shaped NiTiO3 nano-crystalline |
| CN101880870B (en) * | 2010-07-15 | 2012-05-23 | 陕西科技大学 | Preparation method of NiTiO3 thin film |
| CN105032464B (en) * | 2015-07-16 | 2017-07-07 | 湖南大学 | Carbonitride metatitanic acid nickel composite material and preparation method and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2757656C1 (en) * | 2021-02-19 | 2021-10-19 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for obtaining a coating from single-phase nickel titanate on a corundum substrate |
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