CN109824057A - A kind of method of freeze drying technology enhancing montmorillonite surface property - Google Patents
A kind of method of freeze drying technology enhancing montmorillonite surface property Download PDFInfo
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- CN109824057A CN109824057A CN201910039053.7A CN201910039053A CN109824057A CN 109824057 A CN109824057 A CN 109824057A CN 201910039053 A CN201910039053 A CN 201910039053A CN 109824057 A CN109824057 A CN 109824057A
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Abstract
The invention discloses a kind of methods of freeze drying technology enhancing montmorillonite surface property.This method improves the dispersion performance of montmorillonite using freeze drying technology, is then surface modified to enhance stratiform montmorillonite surface property.The montmorillonite with fine dispersion performance is obtained by vacuum freeze drying.By mixing speed, degree of scatter and the freeze-drying time of control montmorillonite in water, the freeze-drying montmorillonite of optimal conditions dispersion is obtained.Freeze-drying montmorillonite is subjected to dopamine surface modification, obtains the montmorillonite of modification.The method of the present invention has the features such as easy to operate, test favorable reproducibility, high-efficient, can get the stratiform montmorillonite that surface has functional group, and for the dispersibility and functionalization for solving inorganic montmorillonite, the compatibility for improving montmorillonite and organic matter provides a kind of new way.
Description
Technical field
The invention belongs to chemical material technical fields, and in particular to a kind of side of freeze drying technology enhancing montmorillonite surface property
Method.
Background technique
Layered clay mineral becomes materialogy and mineralogy is ground because it is with two-dimensional structure and unique interlamination region environment
Study carefully the hot spot in field, research finds that this kind of stratified material limellar stripping, which is become nanoscale twins, has important value
(Science,2013,340(6139):1226419).Layered clay mineral is after layer structure is lifted off of, specific surface area
With cation exchange capacity be significantly increased (Advances in Colloid&Interface Science, 1999,82 (1-3):
43), it can be achieved that material assembles, prepares inorganic non-metallic base new material.Exfoliated lamellar clay gathers in paper industry, fire retardant
The fields such as object nanocomposite are closed to be used widely.
For the expansion layer or lift-off technology of montmorillonite, physical method and chemical method can be used.The physics side generallyd use
Method has ultrasonic method and mechanical attrition method.Ultrasonic treatment is to realize the common physics side of montmorillonite layer removing in organic media
Method can obtain the product (Applied Clay Science, 2006,32 (1-2): 0-146) being partially stripped.Mechanical attrition method
Mainly by " freely the leaving " of the frictional force and ball-milling medium itself generated between ball-milling medium and adjacent layer (liner plate)
Montmorillonite is ground and is smashed (Applied Clay Science, 2014,97-98 (8): 8-16. mining machinery, 2008
(9):74-77).In mechanical milling process, with Ball-milling Time increase the fragmentation and deformation that will lead to part montmorillonite layer
(Applied Clay Science, 2010,47 (3-4): 0-202), is easy to produce sample slimeball and keeps ball action uneven,
Part brought peeling effect after the montmorillonite of dry ball-milling treatment fails to remain imvite modified.
Montmorillonite is more effectively removed to realize, common chemical modification method is to carry out intercalation to montmorillonite.For
Part stratified material can reduce the effect between lamella using this chemical method of graft process in Inter layer adsorption guest molecule method
Power can reduce peel resistance and realize removing (Nature Nanotechnology, 2011,6 (3): 147-150).By chemistry
The montmorillonite of method processing is easier that polymer is convenient for be inserted into, so that polymer phyllosilicate nanocomposite be made.Have
The common modifying agent of machineization processing has alkylammonium class and amino acids.
Cetyl trimethylammonium bromide (CTAB) is intercalator, by the technique of sonic oscillation after first mechanical stirring to sodium
Base montmorillonite is modified, and modified drying and grinding prepares ultra-dispersed montmorillonite.X-ray diffraction (XRD) is the result shows that ultra-dispersed
Cheating engaging layer spacing increases to 3.13nm by 1.01nm before modified, and to be stripped into single lamella, (silicate is logical for montmorillonite
Report, 2009,28 (1): 58-62).Organic composite is carried out to montmorillonite using CTAB and silane coupling agent (KH-560) to be modified, and is led to
It crosses and dries dry gound preparation method and obtain modified montmorillonoid.The modified montmorillonite interlamellar spacing that is averaged increases to from 1.54nm
3.98nm and 2.08nm improves the interfacial effect of montmorillonite and polyvinyl chloride, improves montmorillonite in PVC base system
Dispersing uniformity (apply chemical industry, 2009,38 (6): 827-831).
Freeze Drying Technique is that air pressure is maintained reduced levels using vacuum pump, and water sublimed is promoted to become vapor,
Then by cold trapping, the moisture in sample is removed under sample frozen state.Freeze Drying Technique is able to maintain that montmorillonite is expanded
Layer or the state of removing achieve the effect that layer is expanded in montmorillonite.Dopamine surface aggregate is a kind of novel method of modifying.
(Nature communications,2017,2218.Food Hydrocolloids,2016,61:678-
684.Angewandte Chemie, 2016,55 (9): 3054) dopamine and its derivative due to its auto polymerization and adherency etc. it is special
Property, any material surface (Science, 2007,318,426) can be deposited on by chemical reaction.Promote dopamine in material
Surface aggregate film forming can be modified material surface, and can with the functional group reactions such as amino, sulfydryl, metal ion, it is more
The reactivity of bar amine provides ideal platform for the secondary modification of material surface, for the dispersibility and function for solving montmorillonite
Change, the compatibility for improving montmorillonite and organic matter provides a kind of new way.
Summary of the invention
The present invention is directed in existing organic montmorillonite preparation process, the physical chemistry method of use to montmorillonite expand layer or
Peeling effect has an adverse effect, and provides a kind of method of freeze drying technology enhancing montmorillonite surface property.
To realize the above-mentioned technical purpose, technical solution provided by the invention are as follows:
The method of the freeze drying technology enhancing montmorillonite surface property, includes the following steps:
(1) it disperses montmorillonite high-speed uniform in deionized water and obtains montmorillonite suspension liquid, wherein covered in suspension de-
The concentration of soil is 0.008g/ml to 0.017g/ml；Sub-cloud particulate matter is removed after standing, takes upper layer suspension；Suspension is rotated
It is concentrated by evaporation；Montmorillonite suspension liquid is obtained after concentrate ultrasonic disperse；
(2) montmorillonite suspension liquid is subjected to pre-freeze, pre-freezing temperature is -18 DEG C to -23 DEG C, and the pre-freeze time is 3h to 8h, is made
Suspension sufficiently freezes；The montmorillonite suspension liquid vacuum freeze drying good to pre-freeze is covered de- to get the freeze-drying that surface property enhances
Soil.
Preferably, dispersion revolving speed described in step (1) is 4000rpm to 7000rpm；It is highly preferred that the dispersion turns
Speed is 6000rpm；
Preferably, freeze-drying time described in step (2) is for 24 hours to 60h；It is highly preferred that freeze-drying time is 48h；
The present invention also provides a kind of preparation methods of dopamine surface modification montmorillonite, and the method includes walking as follows
It is rapid:
(1) using tris solution as solvent, Dopamine hydrochloride is that solute is prepared into dopamine solution, is led to
It is 8 to 9.5 that persalt, which adjusts pH value, obtains mixed system A；
(2) the freeze-drying montmorillonite ultrasonic disperse that the present invention obtains is obtained into freeze-drying montmorillonite suspension liquid B in deionized water；
Quickly the resulting mixed system A of step (1) is added in freeze-drying montmorillonite suspension liquid B and carries out high-speed stirred, montmorillonite is lyophilized
Concentration is 0.008g/ml to 0.017g/ml, and it is de- that dopamine surface modification freeze-drying illiteracy is made after washed and vacuum freeze drying
Soil；
Preferably, in step (2), the high-speed stirred revolving speed is 4000rpm to 7000rpm, and temperature is controlled at 25 DEG C
To 45 DEG C, 8h is stirred to react to 32h；It is highly preferred that high-speed stirred revolving speed is 6000rpm, temperature is controlled at 30 DEG C, is stirred to react
24h。
The invention will be further described below:
The present invention provides a kind of methods of freeze drying technology enhancing montmorillonite surface property, and Freeze Drying Technique is applied to
Prepare montmorillonite or modified montmorillonoid.After water is met in montmorillonite, enter hydrone between crystal layer, so that aquation occurs, in exchangeability
Cause the expansion of montmorillonite, the reprimand between montmorillonite crystal layer under the action of cation and hydrogen bond and osmotic pressure and double electrode layer repulsion
Power is greater than its binding strength, so that crystal layer spacing becomes larger.In freeze-drying, the water of piece interlayer is deposited in the form of ice crystal for montmorillonite
With water sublimed, montmorillonite gradually forms loose and porous structure.Enhance montmorillonite layered structure through freeze drying technology of the present invention
Expansion layer or peeling effect after can not only remaining imvite modified, and facilitate further expansion montmorillonite layer spacing；
Meanwhile the method for the present invention to sample almost without loss.The present invention has preparation method simple, tests favorable reproducibility, high-efficient
The features such as.
In short, through freeze drying technology of the present invention treated montmorillonite, be able to maintain that it is imvite modified after dispersion, expand layer or stripping
It is consumed from effect, and to sample nondestructive.The montmorillonite progress DOPA of freeze-drying is amine-modified, and poly-dopamine can not only expand montmorillonite
Piece interlamellar spacing, the dispersion performance of montmorillonite in a polymer matrix can also be improved.Dopamine film thickness can pass through DOPA
Amine concentration, sedimentation time, mixing speed etc. regulate and control, and method is simple and environmentally-friendly, have the features such as test favorable reproducibility, high-efficient,
It is suitble to industrial-scale production, has wide practical use.
Detailed description of the invention
Fig. 1 is the freeze-drying sodium-based montmorillonite (Na-MMT) obtained in an embodiment of the invention；
Fig. 2 is small angle X-ray diffraction (XRD) map of the freeze-drying Na-MMT obtained in an embodiment of the invention；
Fig. 3 is the freeze-drying calcium-base montmorillonite (Ca-MMT) obtained in an embodiment of the invention；
Fig. 4 is the XRD spectrum of the freeze-drying Ca-MMT obtained in an embodiment of the invention；
Fig. 5 is the freeze-drying organic montmorillonite (OMMT) obtained in an embodiment of the invention；
Fig. 6 is the XRD spectrum of the freeze-drying OMMT obtained in an embodiment of the invention；
Fig. 7 is the freeze-drying dopamine sodium-based montmorillonite (PDANa-MMT) obtained in an embodiment of the invention；
Fig. 8 is the electron-microscope scanning figure of the freeze-drying PDANa-MMT obtained in an embodiment of the invention；
Fig. 9 is the XRD spectrum of the freeze-drying PDANa-MMT obtained in an embodiment of the invention；
Figure 10 is the freeze-drying dopamine calcium-base montmorillonite (PDACa-MMT) obtained in an embodiment of the invention；
Figure 11 is the freeze-drying PDACa-MMTXRD map obtained in an embodiment of the invention；
Figure 12 is the freeze-drying dopamine organic montmorillonite (PDA-OMMT) obtained in an embodiment of the invention；
Figure 13 is the electron-microscope scanning figure of the freeze-drying PDA-OMMT obtained in an embodiment of the invention；
Figure 14 is the XRD spectrum of the freeze-drying PDA-OMMT obtained in an embodiment of the invention.
Specific embodiment
Embodiment 1
Na-MMT preparation is lyophilized:
(concentration of Na-MMT is 0.01g/ml), dispersion are dispersed in 300ml deionized water by 3gNa-MMT high-speed uniform
Revolving speed is 6000rpm, removes sub-cloud particulate matter after standing, takes upper layer suspension；Suspension rotary evaporation is concentrated, rotary evaporation
The constant temperature pot temperature of instrument is 65 DEG C, revolving speed 150rpm；Continue ultrasonic disperse, obtains montmorillonite suspension liquid；Montmorillonite is hanged
Supernatant liquid carries out pre-freeze, and pre-freezing temperature is -20 DEG C, and the pre-freeze time is 6h, freezes suspension sufficiently；It is outstanding to the good montmorillonite of pre-freeze
Supernatant liquid vacuum freeze drying is to get freeze-drying Na-MMT.
Fig. 1 is the freeze-drying Na-MMT apparent form figure that the present embodiment obtains, it can be seen from the figure that Na-MMT is in powder
Shape, and Na-MMT is lyophilized in loose sheet.
Fig. 2 is the XRD diffracting spectrum for the freeze-drying Na-MMT that the present embodiment obtains, and can be seen that Na-MMT's from XRD diagram
(001) the corresponding interlamellar spacing d of crystallographic plane diffraction peak001For 1.24nm, (001) crystallographic plane diffraction peak of Na-MMT is bright after freeze-dried processing
Show mobile to small angular direction, interlamellar spacing is expanded to d001=1.27nm illustrates that frozen dried can expand the interlamellar spacing of Na-MMT.
Embodiment 2
Ca-MMT preparation is lyophilized:
(concentration of Ca-MMT is 0.01g/ml), dispersion are dispersed in 300ml deionized water by 3g Ca-MMT high-speed uniform
Revolving speed is 6000rpm, removes sub-cloud particulate matter after standing, takes upper layer suspension；Suspension rotary evaporation is concentrated, rotary evaporation
The constant temperature pot temperature of instrument is 65 DEG C, revolving speed 150rpm；Continue ultrasonic disperse, obtains montmorillonite suspension liquid；Montmorillonite is hanged
Supernatant liquid carries out pre-freeze, and pre-freezing temperature is -20 DEG C, and the pre-freeze time is 6h, freezes suspension sufficiently；It is outstanding to the good montmorillonite of pre-freeze
Supernatant liquid vacuum freeze drying is to get freeze-drying Ca-MMT.
Fig. 3 is the freeze-drying Ca-MMT apparent form figure that the present embodiment obtains, it can be seen from the figure that Ca-MMT is in powder
Shape, and Ca-MMT is lyophilized in loose sheet.
Fig. 4 is the XRD spectrum for the freeze-drying Ca-MMT that the present embodiment obtains, as can be seen that the interlayer of Ca-MMT from XRD diagram
Away from d001=2.31nm, the interlamellar spacing d of Ca-MMT after freeze-drying001It is expanded to 2.34nm, illustrates that frozen dried is conducive to Ca-MMT layers
Expand to spacing.
Embodiment 3
OMMT preparation is lyophilized
(concentration of OMMT is 0.01g/ml) is dispersed in 300ml deionized water by 3gOMMT high-speed uniform, disperses revolving speed
For 6000rpm, sub-cloud particulate matter is removed after standing, takes upper layer suspension；Suspension rotary evaporation is concentrated, Rotary Evaporators
Constant temperature pot temperature is 65 DEG C, revolving speed 150rpm；Continue ultrasonic disperse, obtains montmorillonite suspension liquid；By montmorillonite suspension liquid
Pre-freeze is carried out, pre-freezing temperature is -20 DEG C, and the pre-freeze time is 6h, freezes suspension sufficiently；The montmorillonite suspension liquid good to pre-freeze
Vacuum freeze drying is to get freeze-drying OMMT.
Fig. 5 is the freeze-drying OMMT apparent form figure that the present embodiment obtains, it can be seen from the figure that OMMT is in powdered, and
OMMT is lyophilized in loosely cotton-shaped.
Fig. 6 is the XRD spectrum for the freeze-drying OMMT that the present embodiment obtains, as can be seen that the interlamellar spacing of OMMT from XRD diagram
d001For 2.22nm, the interlamellar spacing d of the OMMT after freeze-drying001It is expanded to 2.29nm, illustrates that frozen dried can expand the layer of OMMT
Spacing.
Embodiment 4
PDANa-MMT preparation is lyophilized
Using tris solution as solvent, 1.4g Dopamine hydrochloride is that solute is prepared into 100ml dopamine
Solution, adjusting pH value by hydrochloric acid is 8.5, obtains mixed system；By 2g freeze-drying Na-MMT ultrasonic disperse in 100ml deionized water
Obtain freeze-drying montmorillonite suspension liquid；Quickly mixed system is added in freeze-drying montmorillonite suspension liquid and carries out high-speed stirred, Na- is lyophilized
The concentration of MMT is 0.01g/ml, and speed of agitator 6000rpm, mixing time is that for 24 hours, temperature is controlled at 30 DEG C；To outstanding after stirring
Supernatant liquid carries out pre-freeze, and pre-freezing temperature is -20 DEG C, and the pre-freeze time is 8h；It will be made after the suspension vacuum freeze drying 48h freezed
The PDANa-MMT of freeze-drying.
Fig. 8 is the freeze-drying PDANa-MMT electron-microscope scanning figure that the present embodiment obtains, it can be seen from the figure that after frozen dried
PDANa-MMT lamella the rolled state of large area is presented, extent of exfoliation obviously increases.
Fig. 9 is the XRD spectrum for the freeze-drying PDANa-MMT that the present embodiment obtains, as can be seen that freeze-drying Na- from XRD diagram
The interlamellar spacing d of MMT001(001) peak freeze-drying PDANa-MMT for 1.27nm, frozen dried is more to small angular variation, after offset
Interlamellar spacing d001It is expanded to 2.40nm, it is obvious to illustrate that the interlamellar spacing that Na-MMT is lyophilized expands layer effect after DOPA is amine-modified.
Embodiment 5
PDACa-MMT preparation is lyophilized
Using tris solution as solvent, 1.4g Dopamine hydrochloride is that solute is prepared into 100ml dopamine
Solution, adjusting pH value by hydrochloric acid is 8.5, obtains mixed system；By 2g freeze-drying Ca-MMT ultrasonic disperse in 100ml deionized water
Obtain freeze-drying montmorillonite suspension liquid；Quickly mixed system is added in freeze-drying montmorillonite suspension liquid and carries out high-speed stirred, Ca- is lyophilized
The concentration of MMT is 0.01g/ml, and speed of agitator 6000rpm, mixing time is that for 24 hours, temperature is controlled at 30 DEG C；To outstanding after stirring
Supernatant liquid carries out pre-freeze, and pre-freezing temperature is -20 DEG C, and the pre-freeze time is 8h；It will be made after the suspension vacuum freeze drying 48h freezed
The PDACa-MMT of freeze-drying.
Figure 11 is the XRD spectrum for the freeze-drying PDACa-MMT that the present embodiment obtains, as can be seen that freeze-drying Ca- from XRD diagram
The interlamellar spacing d of MMT001For 2.34nm, interlamellar spacing d of (001) peak PDACa-MMT of frozen dried to small angular variation, after offset001
It is expanded to 2.72nm, it is obvious to illustrate that the interlamellar spacing that Ca-MMT is lyophilized expands layer effect after DOPA is amine-modified.
Embodiment 6
PDA-OMMT preparation is lyophilized
Using tris solution as solvent, 1.4g Dopamine hydrochloride is that solute is prepared into 100ml dopamine
Solution, adjusting pH value by hydrochloric acid is 8.5, obtains mixed system；By 2g freeze-drying OMMT ultrasonic disperse in 100ml deionized water
To freeze-drying montmorillonite suspension liquid；Quickly mixed system is added in freeze-drying montmorillonite suspension liquid and carries out high-speed stirred, OMMT is lyophilized
Concentration be 0.01g/ml, speed of agitator 6000rpm, mixing time be for 24 hours, temperature control at 30 DEG C；To suspension after stirring
Liquid carries out pre-freeze, and pre-freezing temperature is -20 DEG C, and the pre-freeze time is 8h；Freeze being made after the suspension vacuum freeze drying 48h freezed
Dry PDA-OMMT.
Figure 13 is the freeze-drying PDA-OMMT electron-microscope scanning figure that the present embodiment obtains, it can be seen from the figure that after frozen dried
PDA-OMMT lamella the rolled state of large area is presented, extent of exfoliation obviously increases.
Figure 14 is the XRD spectrum for the freeze-drying PDA-OMMT that the present embodiment obtains, as can be seen that freeze-drying OMMT from XRD diagram
Interlamellar spacing d001(001) peak PDA-OMMT for 2.29nm, frozen dried is more to small angular variation, the interlamellar spacing d after offset001
It is expanded to 2.74nm, it is obvious to illustrate that the interlamellar spacing that OMMT is lyophilized expands layer effect after DOPA is amine-modified.
Claims (10)
1. a kind of method of freeze drying technology enhancing montmorillonite surface property, which is characterized in that described method includes following steps:
(1) it disperses montmorillonite high-speed uniform in deionized water and obtains suspension, sub-cloud particulate matter is removed after standing, takes upper layer
Suspension；Suspension rotary evaporation is concentrated；Montmorillonite suspension liquid is obtained after concentrate ultrasonic disperse；
(2) montmorillonite suspension liquid is subjected to pre-freeze, freezes suspension sufficiently；The montmorillonite suspension liquid vacuum refrigeration good to pre-freeze
The dry freeze-drying montmorillonite enhanced to get surface property.
2. the method as described in claim 1, which is characterized in that dispersion revolving speed described in step (1) be 4000 to
7000rpm。
3. method according to claim 2, which is characterized in that dispersion revolving speed described in step (1) is 6000rpm.
4. the method as described in claim 1, which is characterized in that freeze-drying time described in step (2) is for 24 hours to 60h.
5. method as claimed in claim 4, which is characterized in that freeze-drying time described in step (2) is 48h.
6. the method as described in claim 1, which is characterized in that the concentration of montmorillonite is in step (1) described suspension
0.008g/ml to 0.017g/ml；Pre-freezing temperature described in step (2) is -18 DEG C to -23 DEG C, and the pre-freeze time is 3h to 8h.
7. a kind of preparation method of dopamine surface modification montmorillonite, which is characterized in that the system of the surface modification montmorillonite
Preparation Method includes the following steps:
(1) using tris solution as solvent, Dopamine hydrochloride is that solute is prepared into dopamine solution, passes through salt
It is 8 to 9.5 that acid, which adjusts pH value, obtains mixed system A；
(2) the freeze-drying montmorillonite ultrasonic disperse for obtaining any one of claim 1 to 6 the method obtains in deionized water
Montmorillonite suspension liquid B is lyophilized, quickly the resulting mixed system A of step (1) is added in freeze-drying montmorillonite suspension liquid B and carries out high speed
Stirring after washed and freeze-drying, is made dopamine surface modification and montmorillonite is lyophilized.
8. the method for claim 7, which is characterized in that the resulting mixed system of step (1) is added in step (2) and freezes
When carrying out high-speed stirred in dry montmorillonite suspension liquid, the concentration that montmorillonite is lyophilized is 0.008g/ml to 0.017g/ml.
9. the method for claim 7, which is characterized in that high-speed stirred revolving speed described in step (2) be 4000 to
7000rpm, temperature are controlled at 25 to 45 DEG C, are stirred to react 8 to 32h.
10. method as claimed in claim 9, which is characterized in that high-speed stirred revolving speed described in step (2) is 6000rpm,
Temperature is controlled at 30 DEG C, is stirred to react for 24 hours.
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| CN110240172A (en) * | 2019-07-26 | 2019-09-17 | 沈阳工业大学 | A kind of method that gas phase removing prepares montmorillonite-based nano piece |
| CN111875975A (en) * | 2020-08-24 | 2020-11-03 | 长沙理工大学 | Modified asphalt and application thereof |
| CN112316891A (en) * | 2020-09-22 | 2021-02-05 | 上海傲江生态环境科技有限公司 | Technology for treating polycyclic aromatic hydrocarbon-heavy metal combined polluted soil by utilizing organic modified montmorillonite |
| CN113471530A (en) * | 2021-07-28 | 2021-10-01 | 西安交通大学 | Preparation method and application of inorganic clay array |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240172A (en) * | 2019-07-26 | 2019-09-17 | 沈阳工业大学 | A kind of method that gas phase removing prepares montmorillonite-based nano piece |
| CN110240172B (en) * | 2019-07-26 | 2022-06-24 | 沈阳工业大学 | Method for preparing montmorillonite nanosheet through gas phase stripping |
| CN111875975A (en) * | 2020-08-24 | 2020-11-03 | 长沙理工大学 | Modified asphalt and application thereof |
| CN112316891A (en) * | 2020-09-22 | 2021-02-05 | 上海傲江生态环境科技有限公司 | Technology for treating polycyclic aromatic hydrocarbon-heavy metal combined polluted soil by utilizing organic modified montmorillonite |
| CN113471530A (en) * | 2021-07-28 | 2021-10-01 | 西安交通大学 | Preparation method and application of inorganic clay array |
| CN113471530B (en) * | 2021-07-28 | 2022-10-25 | 西安交通大学 | Preparation method and application of inorganic clay array |
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