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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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title abstract description 5
- 239000000454 talc Substances 0.000 claims abstract description 46
- 229910052623 talc Inorganic materials 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 9
- 150000002815 nickel Chemical class 0.000 claims abstract description 9
- 235000012222 talc Nutrition 0.000 claims description 41
- 239000000047 product Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 230000018044 dehydration Effects 0.000 claims description 11
- 238000006297 dehydration reaction Methods 0.000 claims description 11
- 239000012467 final product Substances 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 11
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 6
- 229940078494 nickel acetate Drugs 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- -1 stearic acid acyloxy titanate esters Chemical class 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 7
- 239000011707 mineral Substances 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 abstract 3
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000004913 activation Effects 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 12
- 239000002250 absorbent Substances 0.000 description 9
- 230000002745 absorbent Effects 0.000 description 8
- 239000011229 interlayer Substances 0.000 description 8
- 239000011358 absorbing material Substances 0.000 description 6
- 230000002687 intercalation Effects 0.000 description 5
- 238000009830 intercalation Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 229910052604 silicate mineral Inorganic materials 0.000 description 2
- 229920000914 Metallic fiber Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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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