CN106517224B - A kind of preparation method of kaolinite nanometer sheet - Google Patents
A kind of preparation method of kaolinite nanometer sheet Download PDFInfo
- Publication number
- CN106517224B CN106517224B CN201611064110.XA CN201611064110A CN106517224B CN 106517224 B CN106517224 B CN 106517224B CN 201611064110 A CN201611064110 A CN 201611064110A CN 106517224 B CN106517224 B CN 106517224B
- Authority
- CN
- China
- Prior art keywords
- kaolinite
- nanometer sheet
- calcined
- preparation
- control agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention discloses a kind of preparation method of kaolinite nanometer sheet.This approach includes the following steps：A1, calcining and activating processing, kaolinite are calcined at a high temperature of 500 800 DEG C, soaking time 14 hours, through the obtained calcined kaolinite that cools；A2, calcined kaolinite obtained by A1 is dispersed in through ultrasound or mechanical agitation in the ethyl alcohol as granule-morphology adjusting control agent, dimethyl sulfoxide (DMSO) or the mixed solution of lithium chloride and water, the mass ratio of the adjusting control agent and water is 1~6：10, the mass ratio of the calcined kaolinite and mixed solution is 1:5~20；It is stirred to react in pressure reaction still 12~48 hours under the conditions of 180~240 DEG C, is separated by solid-liquid separation using centrifuge after cooling down later, then dry, break up, finally obtained kaolinite nanometer sheet.Kaolinite nanometer sheet lamella pattern rule prepared by the present invention, no curling tubulation, lamella size are uniform in size.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of preparation methods of kaolinite nanometer sheet.
Background technology
Kaolinite is one kind 1：The layer silicate mineral of 1 type generally has well-regulated six square pieces layer stacking provisions, base
This film layer unit is made of silicon sun tetrahedron and alumina octahedral, and adjacent sheets are connected by interlayer hydrogen bond, has natural receive
Rice lamellar structure.There is extensive use in fields such as traditional papermaking, filler, ceramics.Since nano material has skin effect,
Small-size effect, quantum size effect and macro quanta tunnel effect etc., and its new features and application effect.Related nanometer kaolinite
The research and preparation of stone are by extensive concern both at home and abroad, in polymers function filler, pharmaceutical carrier, chemical catalysis, life
Object electrode etc. has broad application prospects.
The preparation for processing of nano-kaolinite mainly has：Mechanical crushing method, staging, intercalation-stripping process.Mechanical crushing
The characteristics of mineral lamellar structure is mainly utilized in method, under external force, makes kaolinite Particle Breakage and splitting, but this
Method not only high energy consumption, prolonged impact or grinding being easy that kaolinic laminated structure is made to be destroyed, and are unable to reach and receive
Meter level scale.Kaolin is mainly configured to the slurries of low-solid content by staging in water according to Stoke's falling principle, is sunk
Drop layering obtains ultra-fine kaolin, and this method output capacity is low, and is limited by kaolin starting material particulate thing content.Intercalation-
Stripping process mainly makes kaolinite mineral interlamellar spacing expand using intercalator, weakens interlaminar action, is made by grinding the modes such as stripping, ultrasound
Lamella is peeling-off to prepare nano-kaolinite.Some is by repeatedly replacing intercalation, by kaolinite limellar stripping, but this method one
As can make kaolinite lamella occur curling and form kaolinite madreporic canal, it is difficult to obtain kaolinite nanometer sheet.This method intercalation rate and
Effect differs, and granularity and the pattern variation of product are greatly, it is difficult to control, the recycling of intercalation organic matter is difficult, and production cost is high, the period
It is long.
Invention content
The purpose of the present invention be exactly for the above-mentioned prior art in the presence of shortcoming and provide it is a kind of it is simple for process,
To kaolinite raw type without particular/special requirement, product sheet tactical rule utilizes the kaolinite nanometer that kaolinite is raw material preparation
The method of piece.
The purpose of the present invention can be realized by following technique measures：
The preparation method of the kaolinite nanometer sheet of the present invention includes the following steps：
A1, calcining and activating processing, kaolinite are calcined at a high temperature of 500-800 DEG C, soaking time 1-4 hours,
Through the obtained calcined kaolinite that cools；
A2, by calcined kaolinite obtained by A1 through ultrasound or mechanical agitation be dispersed in the ethyl alcohol as granule-morphology adjusting control agent,
In the mixed solution of dimethyl sulfoxide (DMSO) or lithium chloride and water, the mass ratio of the adjusting control agent and water is 1~6：10, the calcining is high
The mass ratio of ridge stone and mixed solution is 1:5~20；It is stirred to react in pressure reaction still under the conditions of 180~240 DEG C later
It 12~48 hours, is separated by solid-liquid separation using centrifuge after cooling down, then dries, breaks up, finally obtained kaolinite nanometer sheet.
The lamellar spacing of heretofore described kaolinite nanometer sheet is 10~40 nanometers, a diameter of 50~200 nanometers of lamella.
Calcining and activating processing in the present invention described in step A1 is carried out under air or inert gas environment；Using horse
Not stove, rotary kiln or shaft furnace are calcined.
Beneficial effects of the present invention are as follows：
The present invention is calcined using calcining and activating and hydro-thermal Morphological control technology, kaolinite in certain temperature range, brilliant
A degree of destruction can occur for body structure, reduce restriction effect of the lattice to silicon, aluminium atom in kaolinite, make its chemistry
Activity improves.The calcined kaolinite being activated under hydrothermal is easier to that crystallization occurs, in the effect of Morphological control agent
Under, regulate and control crystallization, it is made to be grown in two-dimensional directional, forms kaolinite nanometer sheet.The present invention by after kaolinite calcining and activating,
Under the action of Morphological control agent, only need a hydro-thermal reaction processing that can prepare the intact kaolinite nanometer sheet of laminated structure.
And adjusting control agent and water can recycle after separation of solid and liquid, the environment friendly and pollution-free object discharge of production process.This technology with
Existing method is compared, simple for process, and product pattern laminated structure is intact, kaolinite nanometer sheet lamellar spacing it is small 40 nanometers with
Under, diameter is less than 200 nanometers, it is easy to accomplish industrialized production.
Specific implementation mode
The present invention is further described below with reference to embodiment：
Embodiment 1：
A1, calcining and activating processing, kaolinite powder is placed in Muffle furnace, cold in 600 DEG C of temperature lower calcinations 1.5 hours
But it is collected after cooling down and activation kaolinite powder is made.
A2, with mass ratio be 1:Activation kaolinite powder obtained by A1 is dispersed in as granule-morphology adjusting control agent by 12 ratio
Ethyl alcohol and water mixed solution（Ethyl alcohol is with water quality than 2:10）In, stirring pulping moves into slurries in autoclave,
Under the conditions of 200 DEG C, magnetic agitation is reacted 24 hours, is detached through centrifugal solid-liquid, is dried, broken up under the conditions of 100 DEG C, is made
Kaolinite nanometer sheet.Gained kaolinite nanometer sheet, 36 nanometers of lamella average thickness, lamella average diameter is at 170 nanometers.
Embodiment 2：
A1, calcining and activating processing, kaolinite powder is placed in Muffle furnace, cooling in 700 DEG C of temperature lower calcinations 1 hour
It is collected after cooling and activation kaolinite powder is made.
A2, with mass ratio be 1:Activation kaolinite powder obtained by A1 is dispersed in as granule-morphology adjusting control agent by 10 ratio
Dimethyl sulfoxide (DMSO) and water mixed solution（Dimethyl sulfoxide (DMSO) is with water quality than 3:10）In, stirring pulping moves into slurries high
It presses in reaction kettle, under the conditions of 180 DEG C, magnetic agitation is reacted 36 hours, is detached through centrifugal solid-liquid, is carried out under the conditions of 100 DEG C
Drying, breaks up, and kaolinite nanometer sheet is made.Gained kaolinite nanometer sheet, 30 nanometers of lamella average thickness, lamella average diameter exists
140nm。
Embodiment 3：
A1, calcining and activating processing, kaolinite powder is placed in Muffle furnace, cooling in 600 DEG C of temperature lower calcinations 2 hours
It is collected after cooling and activation kaolinite powder is made.
A2, with mass ratio be 1:Activation kaolinite powder obtained by A1 is dispersed in as granule-morphology adjusting control agent by 8 ratio
Lithium chloride and water mixed solution（Lithium chloride is with water quality than 3:10）In, slurries are moved into autoclave by stirring pulping
Interior, under the conditions of 210 DEG C, magnetic agitation is reacted 48 hours, is detached through centrifugal solid-liquid, is dried, beaten under the conditions of 100 DEG C
It dissipates, kaolinite nanometer sheet is made.Gained kaolinite nanometer sheet, 20 nanometers of lamella average thickness, lamella average diameter is in 120nm.
The method have the characteristics that using calcining and activating and Morphological control technology, prepares kaolinite through a hydro-thermal reaction and receive
Rice piece, simple for process, reaction speed is fast, adjusting control agent and the recyclable recycling of water.Calcining and activating is being carried out to kaolinite first
Processing, then carries out heating reaction, most afterwards through centrifugal solid-liquid with water and Morphological control agent mixed pulp in autoclave
Separation, it is dry, break up, both kaolinite nanometer sheet of the present invention.
Claims (3)
1. a kind of preparation method of kaolinite nanometer sheet, it is characterised in that：It the described method comprises the following steps：
A1, calcining and activating processing, kaolinite are calcined at a high temperature of 500-800 DEG C, soaking time 1-4 hours, through cold
But cool down and calcined kaolinite is made；
A2, calcined kaolinite obtained by A1 is dispersed in the ethyl alcohol as granule-morphology adjusting control agent, diformazan through ultrasound or mechanical agitation
In the mixed solution of base sulfoxide or lithium chloride and water, the mass ratio of the adjusting control agent and water is 1~6：10, the calcined kaolinite
Mass ratio with mixed solution is 1:5~20；It is stirred to react 12 in pressure reaction still under the conditions of 180~240 DEG C later~
It 48 hours, is separated by solid-liquid separation using centrifuge after cooling down, then dries, breaks up, finally obtained kaolinite nanometer sheet.
2. the preparation method of kaolinite nanometer sheet according to claim 1, it is characterised in that：The kaolinite nanometer sheet
Lamellar spacing is 10~40 nanometers, a diameter of 50~200 nanometers of lamella.
3. the preparation method of kaolinite nanometer sheet according to claim 1, it is characterised in that：Calcining described in step A1
Activation process is carried out under air or inert gas environment；It is calcined using Muffle furnace, rotary kiln or shaft furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064110.XA CN106517224B (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of kaolinite nanometer sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064110.XA CN106517224B (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of kaolinite nanometer sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106517224A CN106517224A (en) | 2017-03-22 |
| CN106517224B true CN106517224B (en) | 2018-09-18 |
Family
ID=58357702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611064110.XA Active CN106517224B (en) | 2016-11-28 | 2016-11-28 | A kind of preparation method of kaolinite nanometer sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517224B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336125A (en) * | 2018-12-14 | 2019-02-15 | 河南理工大学 | A kind of preparation method of the kaolinite microballoon of nanometer of hierarchical structure |
| CN112246215A (en) * | 2020-11-04 | 2021-01-22 | 河南理工大学 | Method for preparing adsorbing material for water treatment by using coal gangue as raw material |
| CN115322611A (en) * | 2022-08-25 | 2022-11-11 | 广东省水利水电科学研究院 | Lamellar kaolin material and preparation method and application thereof |
| CN116042085A (en) * | 2023-02-20 | 2023-05-02 | 江苏富乐华功率半导体研究院有限公司 | Composite material for improving partial discharge performance of ceramic substrate, preparation process and application method |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513800A (en) * | 2003-03-07 | 2004-07-21 | 广东佛陶集团物资工贸有限公司 | Manufacturing method of nano-kaolin |
| CN101058425A (en) * | 2006-04-21 | 2007-10-24 | 同济大学 | Method for preparing nano-grade sheet kaolinite |
| CN100569868C (en) * | 2006-08-09 | 2009-12-16 | 河北工程大学 | Nano stripping method for coal series hard kaolinite |
| CN102205971B (en) * | 2010-03-31 | 2013-05-01 | 中国科学院过程工程研究所 | Method for preparing nano-sized kaolinite |
| CN102602951B (en) * | 2012-03-22 | 2013-07-24 | 天津大学 | Method for preparing kaoline nanotube |
-
2016
- 2016-11-28 CN CN201611064110.XA patent/CN106517224B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106517224A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106517224B (en) | A kind of preparation method of kaolinite nanometer sheet | |
| Zhang et al. | Synthesis of lignin-modified silica nanoparticles from black liquor of rice straw pulping | |
| CN107043113B (en) | A kind of method of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam | |
| CN101475222B (en) | Iron oxide hollow microsphere and preparation thereof | |
| CN106540733B (en) | A method of preparing graphite phase carbon nitride material | |
| CN112300602A (en) | Modification method of inorganic filler | |
| CN104016408B (en) | A kind of synthetic method of sodium niobate nano line | |
| CN101823723B (en) | Process method for preparing ultra-fine high-brightness sericite powder by pyrophyllite | |
| CN106477605A (en) | A kind of method preparing alumina hollow ball | |
| CN106622331A (en) | Preparation method of high-specific-surface-area graphite phase carbon nitride photocatalyst | |
| CN103232049A (en) | Preparation method of alpha-Al2O3 cage-structure hollow microspheres | |
| Yang et al. | Comparison of the microwave and conventional sintering of Li2TiO3 ceramic pebbles | |
| CN102674381A (en) | Method for preparing nano mullite powder from coal-based kaolin | |
| CN107716002A (en) | The apparatus and method that a kind of pure shear ball milling prepares hexagonal boron nitride nanosheet with supersonic synergic | |
| CN103274672B (en) | Preparation method for alumina hollow spheres | |
| CN104743562A (en) | Preparation method of sericite nanosheets | |
| CN104229850A (en) | Method and device for producing nano calcium carbonate by microwave drying | |
| CN108557863A (en) | A kind of preparation method of lanthana | |
| CN108502856A (en) | A kind of green economy preparation method of two dimension carbonitride | |
| CN106186013B (en) | A kind of method that use rheological phase reaction method synthesizes flower ball-shaped meso-porous alumina | |
| CN105884372B (en) | Organic network method synthesizes AlN ceramic powder method | |
| CN104760966B (en) | A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate | |
| Xu et al. | Stability of the compounds obtained by intercalating potassium acetate molecules into kaolinite from coal measures | |
| CN102205971B (en) | Method for preparing nano-sized kaolinite | |
| CN101654280A (en) | Preparation method of titanium dioxide nano powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190618 Address after: 214400 Fengming Road, Huangtang, Xuxiake Town, Jiangyin City, Wuxi City, Jiangsu Province Patentee after: Wuxi Feiler Powder Material Co., Ltd. Address before: 454003 No. 2001 Century Avenue, Jiaozuo high tech Zone, Henan Patentee before: Henan Polytechnic University |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 214400 Fengming Road, Huangtang, Xuxiake Town, Jiangyin City, Wuxi City, Jiangsu Province Patentee after: Wuxi Feile high performance materials Co., Ltd Address before: 214400 Fengming Road, Huangtang, Xuxiake Town, Jiangyin City, Wuxi City, Jiangsu Province Patentee before: Wuxi Feiler Powder Material Co., Ltd. |