CN109133077A - A method of preparing two-dimentional nearly single layer montmorillonite - Google Patents
A method of preparing two-dimentional nearly single layer montmorillonite Download PDFInfo
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- CN109133077A CN109133077A CN201810924293.0A CN201810924293A CN109133077A CN 109133077 A CN109133077 A CN 109133077A CN 201810924293 A CN201810924293 A CN 201810924293A CN 109133077 A CN109133077 A CN 109133077A
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- montmorillonite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- 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
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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
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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
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Abstract
The present invention relates to a kind of methods for preparing two-dimentional nearly single layer montmorillonite, and powdered sodium monotmorillonite is added in pure water and is stirred to being completely dispersed, montmorillonite suspension is obtained；Ultrasound or stir process are carried out to montmorillonite suspension, are then centrifuged for taking upper layer suspension；Upper layer suspension is subjected to vacuum freeze drying, obtains the nearly single layer montmorillonite sample of white cotton shape two dimension, as product.Compared with prior art, preparation method is simple by the present invention, reproducible, and obtained nearly single layer montmorillonite property is stablized, and can be produced in enormous quantities.For adsorbent, germ killing drugs, dielectric, catalyst carrier etc..
Description
Technical field
The present invention relates to the preparation methods of nano material, more particularly, to a kind of side for preparing two-dimentional nearly single layer montmorillonite
Method.
Background technique
Natural bulk montmorillonite is the mineral material with layer structure, and surface is negatively charged, passes through model moral between layers
There is the metal cation (Na for maintaining charge balance in magnificent power connection, interlayer+、K+、Ca2+Deng).In recent years, with graphene, C3N4
The rise of the nearly single layer nano material of New Two Dimensionals is waited, montmorillonite type hydroxide two-dimension nano materials also start to be paid close attention to.This
Before, the design feature based on natural smectite, Cui et al. makes surfactant enter montmorillonite layer by cationic exchange interaction
Between, nearly single layer montmorillonite is then prepared by click chemistry method.Yan etc. uses Na between CTAB and montmorillonite layer+Exchange, then lead to
It crosses ball-milling method and obtains nearly single layer montmorillonite.Surfactant used in nearly single layer montmorillonite method made above, it is more difficult to biology
Degradation, may have an adverse effect to water environment or groundwater environment.And physical method is used to prepare the nearly single layer montmorillonite of two dimension, then
It can avoid introducing other substances in preparation process, simplify preparation process and environmental-friendly.Therefore the present invention, which will be conceived to, utilizes sodium
The environment-friendly preparation method thereof of the nearly single layer nano material of type montmorillonite preparation two dimension.Based on this, it is close that we have developed a kind of acquisition two dimension
The new way of single layer montmorillonite.The nearly single layer montmorillonite average grain diameter of gained is 210 ± 125 nanometers, and average thickness is 2.5 ± 1.0
Nanometer.This nearly single layer structure preparation method is reported for the first time, can be prepared on a large scale two-dimentional montmorillonite, is expected to obtain and be answered extensively
With.
China's montmorillonite rich reserves are explored the preparation method of the nearly single layer montmorillonite of two dimension, can not only be enriched and perfect
The preparation process of montmorillonite can also obtain the product with special construction and excellent performance simultaneously, this is for expanding montmorillonite
Application field and prospect are of great significance.
Summary of the invention
The object of the invention is to deposit to overcome existing base exchange method to prepare the nearly single layer montmorillonite technology of two dimension
Defect, a kind of method of simple and easy, inexpensive nearly single layer montmorillonite of preparation two dimension is provided.
The purpose of the present invention can be achieved through the following technical solutions:
A method of two-dimentional nearly single layer montmorillonite is prepared, using following steps:
(1) powdered sodium monotmorillonite is added in pure water and is stirred to being completely dispersed, obtain montmorillonite suspension；
(2) ultrasound or stir process are carried out to montmorillonite suspension, is then centrifuged for taking upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, obtains the nearly single layer montmorillonite sample of white cotton shape two dimension, i.e.,
For product, microstructure is the nearly single-layer sheet of two-dimensional ultrathin, and hydrodynamic radius is 342 ± 45 nanometers, and partial size is received for 230 ± 125
Rice, with a thickness of 2.5 ± 1.0 nanometers.
Mixing control revolving speed is 50-200rpm in step (1).
When step (2) is ultrasonically treated, the probe of Ultrasonic Cell Disruptor is placed in montmorillonite suspension, controls supersonic frequency
Rate is 90-200W, and ultrasonic time is -240 minutes 10 minutes, and during preparing the nearly single layer montmorillonite of two dimension, supersonic frequency is got over
The yield of height, two-dimentional montmorillonite is higher；Ultrasonic time increased to 240 minutes from 10 minutes, and the yield of two-dimentional montmorillonite is from 38%
57% is increased to, continue to improve supersonic frequency or extends ultrasonic time, superpower energy will lead to two-dimentional montmorillonite and lose two dimension
Structure becomes dotted material.
When step (2) is stirred, control stirring rate is 200rpm-1500rpm, the revolving speed in whipping process from
200rpm increases to 1500rpm, and the yield for stirring 1-7 days two-dimentional montmorillonites increases to 37% from 23%, especially in 500rpm
Under revolving speed, to stirring 3 days, the yield of two-dimentional montmorillonite increased to 31% from 24%, further with mixing time within 1 day for stirring
Increase, the yield of two-dimentional montmorillonite is held essentially constant.
The revolving speed of centrifugal treating is 5000-10000rpm in step (2), and centrifugation time is 10-30 minutes.
Vacuum freeze drying in step (3), vacuum drying temperature are -50 DEG C, drying time 24-72h.
Compared with prior art, the invention is simple and feasible, reproducible, and obtained sheet montmorillonite property is stablized, can be into
Row is produced in enormous quantities, and adsorbent, catalyst carrier, bacteria remover etc. are used as.
Detailed description of the invention
Fig. 1 is the nearly single layer montmorillonite AFM figure of two dimension being prepared.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
1 gram of powdered sodium monotmorillonite is added in 100 milliliters of pure water, control revolving speed is that 200rpm is stirred 45 minutes, is obtained
To uniformly mixed montmorillonite suspension；The probe of Ultrasonic Cell Disruptor is placed in homogeneous solution, ultrasound 30 minutes will then surpass
Montmorillonite suspension after sound is centrifuged 10 minutes under 8000rpm revolving speed, takes upper layer suspension.Then upper layer suspension is freezed
It is dry, obtain the nearly single layer montmorillonite of solid two dimension, as product.The product is nearly single layer montmorillonite, and average grain diameter is received for 230
Rice, average thickness are 2.5 nanometers, and AFM figure is as shown in Figure 1.It can be seen from the figure that obtained two-dimentional montmorillonite product is equal
Even sheet, thickness are about 1.5 nanometers.
Embodiment 2
1 gram of powdered sodium monotmorillonite being added in 100 milliliters of pure water, control revolving speed is that 200rpm is stirred 120 minutes,
Obtain uniformly mixed montmorillonite suspension；The probe of Ultrasonic Cell Disruptor is placed in homogeneous solution, ultrasound 10 minutes, then will
Montmorillonite suspension after ultrasound is centrifuged 10 minutes under 8000rpm revolving speed, takes upper layer suspension.Then upper layer is suspended liquid cooling
It is lyophilized dry, obtains the nearly single layer montmorillonite of solid two dimension, as product.The product is nearly single layer montmorillonite, and average grain diameter is received for 230
Rice, average thickness are 2.5 nanometers.
Embodiment 3
1 gram of powdered sodium monotmorillonite is added in 100 milliliters of pure water, control revolving speed is that 200rpm is stirred 45 minutes, is obtained
To uniformly mixed montmorillonite suspension；Uniformly mixed montmorillonite suspension is continuously stirred 3 days under 500rpm revolving speed,
The montmorillonite suspension after stirring is centrifuged 10 minutes under 8000rpm revolving speed then, takes upper layer suspension；Finally upper layer is hanged
Supernatant liquid freeze-drying obtains the nearly single layer montmorillonite of solid two dimension, as product.The product is nearly single layer montmorillonite, average grain diameter
It is 230 nanometers, average thickness is 2.5 nanometers.
Embodiment 4
1 gram of powdered sodium monotmorillonite is added in 100 milliliters of pure water, control revolving speed is that 200rpm is stirred 45 minutes, is obtained
To uniformly mixed montmorillonite suspension；Uniformly mixed montmorillonite suspension is continuously stirred 3 under 1500rpm revolving speed
Montmorillonite suspension after stirring, is then centrifuged 10 minutes under 8000rpm revolving speed, takes upper layer suspension by it；It finally will be upper
Layer suspension freeze-drying obtains the nearly single layer montmorillonite of solid two dimension, as product.The product is nearly single layer montmorillonite, average
Partial size is 230 nanometers, and average thickness is 2.5 nanometers.
Embodiment 5
A method of two-dimentional nearly single layer montmorillonite is prepared, using following steps:
(1) powdered sodium monotmorillonite is added in pure water, control revolving speed is that 50rpm is stirred to being completely dispersed, and is covered
De- stone suspension；
(2) montmorillonite suspension is ultrasonically treated, the probe of Ultrasonic Cell Disruptor is placed in montmorillonite suspension, controlled
Supersonic frequency processed is 90W, and ultrasound 240 minutes, then controlling revolving speed is that 5000rpm is centrifuged 30 minutes, takes upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, control vacuum drying temperature is -50 DEG C, and the time is for 24 hours, to obtain
To the nearly single layer montmorillonite sample of white cotton shape two dimension, as product, microstructure are the nearly single-layer sheet of two-dimensional ultrathin, average hydrodynamic(al)
Mechanics radius is about 342 nanometers, and average grain diameter is about 230 nanometers, and average thickness is about 2.5 nanometers.
Embodiment 6
A method of two-dimentional nearly single layer montmorillonite is prepared, using following steps:
(1) powdered sodium monotmorillonite is added in pure water, control revolving speed is that 200rpm is stirred to being completely dispersed, and is covered
De- stone suspension；
(2) montmorillonite suspension is ultrasonically treated, the probe of Ultrasonic Cell Disruptor is placed in montmorillonite suspension, controlled
Supersonic frequency processed is 200W, and ultrasound 10 minutes, then controlling revolving speed is that 8000rpm is centrifuged 20 minutes, takes upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, control vacuum drying temperature is -50 DEG C, and time 36h is obtained
To the nearly single layer montmorillonite sample of white cotton shape two dimension, as product, microstructure are the nearly single-layer sheet of two-dimensional ultrathin, average hydrodynamic(al)
Mechanics radius is about 297 nanometers, and average grain diameter is about 105 nanometers, and average thickness is about 1.5 nanometers.
Embodiment 7
A method of two-dimentional nearly single layer montmorillonite is prepared, using following steps:
(1) powdered sodium monotmorillonite is added in pure water, control revolving speed is that 100rpm is stirred to being completely dispersed, and is covered
De- stone suspension；
(2) montmorillonite suspension is stirred, control mixing speed is 200rpm, is stirred 7 days, then control turns
Speed is that 8000rpm is centrifuged 20 minutes, takes upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, control vacuum drying temperature is -50 DEG C, and time 36h is obtained
To the nearly single layer montmorillonite sample of white cotton shape two dimension, as product, microstructure are the nearly single-layer sheet of two-dimensional ultrathin, average hydrodynamic(al)
Mechanics radius is about 387 nanometers, and average grain diameter is about 355 nanometers, and average thickness is about 3.5 nanometers.
Embodiment 8
(1) powdered sodium monotmorillonite is added in pure water, control revolving speed is that 100rpm is stirred to being completely dispersed, and is covered
De- stone suspension；
(2) montmorillonite suspension is stirred, control mixing speed is 1500rpm, stirs 1 day, then controls
Revolving speed is that 10000rpm is centrifuged 10 minutes, takes upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, control vacuum drying temperature is -50 DEG C, and time 72h is obtained
To the nearly single layer montmorillonite sample of white cotton shape two dimension, as product, microstructure are the nearly single-layer sheet of two-dimensional ultrathin, average grain diameter
About 300 nanometers, average thickness is about 2.5 nanometers.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (7)
1. a kind of method for preparing two-dimentional nearly single layer montmorillonite, which is characterized in that this method uses following steps:
(1) powdered sodium monotmorillonite is added in pure water and is stirred to being completely dispersed, obtain montmorillonite suspension；
(2) ultrasound or stir process are carried out to montmorillonite suspension, is then centrifuged for taking upper layer suspension；
(3) upper layer suspension is subjected to vacuum freeze drying, obtains the nearly single layer montmorillonite sample of white cotton shape two dimension, as produces
Product.
2. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that step (2) into
When row ultrasonic treatment, the probe of Ultrasonic Cell Disruptor is placed in montmorillonite suspension, control supersonic frequency is 90W-200W, ultrasound
Time is -240 minutes 10 minutes.
3. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that step (2) into
When row stir process, control stirring rate is 200rpm-1500rpm, is stirred 1-7 days.
4. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that in step (2)
The revolving speed of centrifugal treating is 5000-10000rpm, and centrifugation time is 10-30 minutes.
5. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that in step (1)
Mixing control revolving speed is 50-200rpm.
6. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that in step (3)
Vacuum freeze drying is carried out, vacuum drying temperature is -50 DEG C, and drying time is 24-72 hours.
7. a kind of method for preparing two-dimentional nearly single layer montmorillonite according to claim 1, which is characterized in that be prepared
The microstructure of product is the nearly single-layer sheet of two-dimensional ultrathin, and partial size is 230 ± 125 nanometers, with a thickness of 2.5 ± 1.0 nanometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650400A (en) * | 2019-01-30 | 2019-04-19 | 中国地质大学（武汉） | A kind of DMF intercalation-removing na-montmorillonite ultrathin nanometer piece and preparation method thereof |
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| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
| CN104071798A (en) * | 2014-07-03 | 2014-10-01 | 中国科学院上海硅酸盐研究所 | Ultrathin montmorillonite nanosheet as well as preparation method and application thereof |
| CN107353422A (en) * | 2017-03-29 | 2017-11-17 | 东北大学 | A kind of preparation method of the alkaline negative ion exchange composite film of high inorganics doped amount |
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2018
- 2018-08-14 CN CN201810924293.0A patent/CN109133077A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771517A (en) * | 2014-01-17 | 2014-05-07 | 哈尔滨工业大学 | Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets |
| CN104071798A (en) * | 2014-07-03 | 2014-10-01 | 中国科学院上海硅酸盐研究所 | Ultrathin montmorillonite nanosheet as well as preparation method and application thereof |
| CN107353422A (en) * | 2017-03-29 | 2017-11-17 | 东北大学 | A kind of preparation method of the alkaline negative ion exchange composite film of high inorganics doped amount |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650400A (en) * | 2019-01-30 | 2019-04-19 | 中国地质大学（武汉） | A kind of DMF intercalation-removing na-montmorillonite ultrathin nanometer piece and preparation method thereof |
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