CN107244676B - A kind of method of alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju - Google Patents
A kind of method of alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju Download PDFInfo
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- CN107244676B CN107244676B CN201710435269.6A CN201710435269A CN107244676B CN 107244676 B CN107244676 B CN 107244676B CN 201710435269 A CN201710435269 A CN 201710435269A CN 107244676 B CN107244676 B CN 107244676B
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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
- C01B33/40—Clays
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
The invention discloses the methods of alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju a kind of, specifically attapulgite suspension is placed in alternating electric field, electrically charged Features of Attapulgite Minerals crystalline substance beam or aggregate particle is set to generate relative motion, to generate shearing force overcome aggregation medium rod crystalline substance between electrostatic force or Van der Waals force, attapulgite stick crystalline substance beam and aggregation are depolymerized to the nanometer rods of high degree of dispersion.The present invention makes Features of Attapulgite Minerals crystalline substance beam and aggregation depolymerization using the impulse action that alternating electric field generates, and the loss of stick crystalline substance draw ratio is small, and dispersion effect is good, and product reaches nano-dispersion truly；Entire technical process is without using the harsh conditions such as high temperature, high pressure, easy to operate, at low cost, favorable reproducibility, safety non-pollution；The depolymerization of aggregation and degree of scatter can be controlled by adjusting electric field strength and frequency, and good product performance is at low cost, can be used for the multiple fields such as plastics, rubber, catalyst, petrochemical industry, environmental protection, functional material.
Description
Technical field
The present invention relates to the methods of alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju a kind of, belong to natural non-metallic mine
Deep processing and technical field of nanometer material preparation.
Background technique
Attapulgite also known as palygorskite or Palygorskite, be it is a kind of have layer chain structure, nanoclub-like crystal form and
The aqueous rich magnesium aluminosilicate clays mineral of nano pore.Due to unique nanoclub-like crystal structure and surface nature,
Therefore show excellent colloid, absorption, carrier and reinforcing property, fine chemistry industry, petrochemical industry, decoloration, building materials, environmental protection and
It is applied widely in the fields such as functional material.However, the attapulgite stick intergranular of natural output is since there are stronger models
De Huali and power the effects of hydrogen bond, therefore stick crystalline substance mainly exists with stable stick crystalline substance beam and aggregate form, limits concave convex rod
The application of stone nano ZnO.China's attapulgite resource reserve accounts for more than half of world's total amount, but due to stick crystalline substance beam solution
Poly- critical bottleneck technology never makes a breakthrough, so added value of product is low at present always based on low-end applications, it is serious to make
The development of the China Yue Liao attapulgite industry.
Currently, mainly improving the service performance of attapulgite using various purifications and modified method.
CN102874826A discloses a kind of method of purification of attapulgite, specifically by attapulgite clay be dispersed in water slurrying,
Activator activation is added, sour removal of impurities, ageing, gravitational settling, repeatedly centrifuge separation is added, it is glutinous to finally obtain purification attapulgite
Soil.CN 103738975A discloses a kind of method of purification of attapulgite clay, using slurrying-plus activator-ageing-sedimentation-
Separation and etc. improve the purity of attapulgite.Purification processes can reduce miscellaneous mineral content to a certain extent, improve concave-convex
The deficiencies of purity of stick stone improves service performance, but there is also complex process, the energy consumption of at high cost, water consumption, and activator can also
Cause environmental pollution.Although with various physical methods (CN104014299A) or chemical modification method (CN 102527325A；
CN102553519A；CN 103611494A；CN102247807A；103723785A) the performance of Lai Tigao attapulgite, but it is recessed
The nano ZnO of convex stick stone itself does not still give full play of.
The method for usually improving attapulgite stick crystalline substance dispersion performance mainly has dry and wet.Dry method such as ball milling, superfine powder
It is broken, mill, the advantages that have that easy to operate, yield is high, equipment requirement is low etc., therefore be widely used always.But dry method depolymerization
It is inefficient, and need stronger mechanicals efforts that can damage stick crystalline substance.In recent years, wet process dissociation technique receives more passes
Note, shows depolymerization efficiency more better than dry method.
Alternating electric field is aggregation dispersion new technology developed in recent years, has been used to removing preparing graphite alkene
(CN103253654A).Under action of alternative electric field, size and electrically charged different particles alternating movement in different directions,
Mutually shearing and collision are generated in direction of an electric field variation, to make aggregation and crystalline substance Shu Xieju and scatter.But at present with friendship
Changed electric field depolymerization attapulgite clay stick crystalline substance beam and aggregation also have no the precedent of application there are no correlative study report.
Summary of the invention
It is an object of the invention to: the method for alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju a kind of is provided, it is intended to
The dissociation efficiency of Features of Attapulgite Minerals crystalline substance beam is improved, the loss of stick crystalline substance draw ratio in depolymehzation process is reduced, prepares dispersibility
1-dimention nano attapulgite material good, draw ratio is high.
The present invention utilizes the principle of colloid chemistry and electrokinetics, realizes Features of Attapulgite Minerals crystalline substance beam and aggregation in alternation electricity
Efficient depolymerization in.Specifically attapulgite suspension is placed in alternating electric field, makes aggregate particle in action of alternative electric field
Lower movement.Since different sizes, electrically charged different particle movement rate under the action of alternating electric field have differences, institute
Can produce stronger collision and shearing, aggregation depolymerization becomes small brilliant beam, brilliant beam is finally made to be depolymerized to receiving for high degree of dispersion
Rice attapulgite.
The method that the alternating electric field of the invention induces Features of Attapulgite Minerals crystalline substance Shu Xieju is by attapulgite raw ore by broken
It is broken, to roller extrusion process after, be distributed to be made in the aqueous solution containing chemical assistant mass concentration be 5 ~ 20% suspension, then
It is transferred to two sides to be equipped in the slot type receptacles of electrode, and applies alternating current at electrode both ends, handle 10 ~ 60 min, then machinery stirs
25 ~ 30 min of dispersion is mixed, then applies alternating electric field and handles 30 ~ 120 min；Then by suspension cyclone classification remove quartz sand and
Large granular impurity most obtains the nano-attapulgite stone of high degree of dispersion through separation, drying, crushing afterwards.
Attapulgite purity should be greater than 85%.
The voltage of alternating current is 100 ~ 380 V, and frequency is 50 ~ 1200Hz；Alternating electric field intensity is 500 ~ 2000 V/m.
Chemical assistant is one of glycine, alanine, diammonium hydrogen phosphate, ammonium dihydrogen phosphate and ammonium phosphate, and chemistry helps
The mass concentration of agent aqueous solution is 0.1 ~ 2.5%.The effect of addition chemical assistant is that regulation attapulgite Particle surface charge is close
Degree, improves its locomitivity in impulse electric field.
The structural characterization of product of the present invention: it is confirmed by X-ray powder diffraction (XRD) and scanning electron microscope (SEM)
Attapulgite depolymerization front-end geometry and metamorphosis.Fig. 1 is attapulgite raw ore (i) and present invention process prepares nano-attapulgite
The XRD spectrum of stone (ii).It will be seen from figure 1 that mainly there is the characteristic peak of attapulgite and quartz in attapulgite clay, pass through
After present invention process processing, there is no significant changes for attapulgite characteristic peak, but the characteristic diffraction peak of quartz almost disappears, and says
Bright present invention process also eliminates quartz sand impurity during depolymerization attapulgite crystalline substance beam.Fig. 2 attapulgite raw ore (a),
Present invention process prepares nano-attapulgite stone (b) and schemes to roller+high speed machine stir process attapulgite (c) SEM.From Fig. 2
As can be seen that attapulgite be nano bar-shape structure, but in raw ore attapulgite stick crystalline substance with the aggregation and crystalline substance of dense packing
Beam form exists, and the nano stick crystal of independent dispersion is not observed.After present invention process is handled, attapulgite crystalline substance beam and poly-
Collective disappears, and has the nanometer rods of a large amount of independent dispersions to occur, illustrates that attapulgite crystalline substance beam and aggregation are depolymerizated and are dispersed into list
Dispersed attapulgite nano stick crystal.Extraordinary dispersion is presented by the nano-attapulgite stone that depolymerization obtains, and stick crystalline substance is long
Spend no significant change compared with raw ore medium rod crystalline substance length.It can be seen that present invention process preparation by comparison diagram 2b and Fig. 2 c
Nano-attapulgite stone it is more preferable to the attapulgite dispersibility of roller+high speed machine stirring technique preparation than traditional.
The present invention has the advantage that compared with the prior art
1, the present invention makes Features of Attapulgite Minerals crystalline substance beam and aggregation depolymerization using the impulse action that alternating electric field generates, therefore
The loss of stick crystalline substance draw ratio is small, and dispersion effect is good, and product reaches nano-dispersion truly；
2, entire technical process is without using the harsh conditions such as high temperature, high pressure, easy to operate, at low cost, favorable reproducibility, safety
It is pollution-free；
3, the depolymerization of aggregation and degree of scatter can be controlled by adjusting electric field strength and frequency, properties of product
It is good, it is at low cost, it can be used for the multiple fields such as plastics, rubber, catalyst, petrochemical industry, environmental protection, functional material.
Detailed description of the invention
Fig. 1 is the XRD spectrum that attapulgite raw ore and present invention process prepare nano-attapulgite stone.
Fig. 2 is attapulgite raw ore and present invention process prepares nano-attapulgite stone and to roller+high-speed stirred processing bumps
The SEM of stick stone schemes.
Specific embodiment
Below by flat specific embodiment to the alternating electric field of the invention induction Features of Attapulgite Minerals crystalline substance Shu Xieju method and
Effect is described further.
Embodiment 1
By attapulgite raw ore by it is broken, to roller extrusion process after, take 1kg to be distributed to 20 kg mass concentrations 0.1%
The suspension that concentration is 5% is made in glycine solution, is then transferred to two sides equipped in the container of electrode, is applied at electrode both ends
Add the alternating current of 380V and 50 Hz, handles 10 min, mechanical stirring disperses 30 min, then applies 2000 V/m's of electric field strength
Alternating electric field handles 30 min；Then suspension cyclone classification is removed into quartz sand and large granular impurity, finally carries out filters pressing point
From, dry and pulverization process, the nano-attapulgite stone of high degree of dispersion is obtained.Gained nano-attapulgite stone is distributed to water with 20%
When middle, concave convex rod stone grain diameter D90≤1 micron in suspension, attapulgite stick crystalline substance draw ratio >=32.Nano-attapulgite stone 7%
Water slurry viscosity is 3460 mPa.s, reaches 6.76 times of raw ore suspension viscosity (512 mPa.s).
Embodiment 2
By attapulgite raw ore by it is broken, to roller extrusion process after, take 1kg to be distributed to 5 kg mass concentrations 2.5%
The suspension that concentration is 20% is made in ammonium phosphate solution, is then transferred to two sides equipped in the container of electrode, is applied at electrode both ends
Add the alternating current of 100V and 1200 Hz, handles 60 min, mechanical stirring disperses 30 min, then applies 500 V/m's of electric field strength
Alternating electric field handles 120 min；Then suspension cyclone classification is removed into quartz sand and large granular impurity, finally carries out filters pressing point
From, dry and pulverization process, the nano-attapulgite stone of high degree of dispersion is obtained.Gained nano-attapulgite stone is distributed to water with 20%
When middle, concave convex rod stone grain diameter D90≤1.2 micron in suspension, attapulgite stick crystalline substance draw ratio >=31.Nano-attapulgite stone
7% water slurry viscosity is 3270 mPa.s, reaches 6.39 times of raw ore suspension viscosity (512 mPa.s).
Embodiment 3
By attapulgite raw ore by it is broken, to roller extrusion process after, take 1kg to be distributed to 10 kg mass concentrations 1% the third
The suspension that concentration is 10% is made in propylhomoserin aqueous solution, is then transferred to two sides equipped in the container of electrode, applies at electrode both ends
The alternating current of 220V and 500 Hz handle 60 min, and mechanical stirring disperses 30 min, then applies 1000 V/m alternation of electric field strength
Then suspension cyclone classification is removed quartz sand and large granular impurity by 60 min of electric field treatment, finally carry out filters pressing separation, do
Dry and pulverization process obtains the nano-attapulgite stone of high degree of dispersion.When gained nano-attapulgite stone is distributed in water with 20%, hang
Concave convex rod stone grain diameter D90≤1.3 micron in supernatant liquid, attapulgite stick crystalline substance draw ratio >=33.7% water of nano-attapulgite stone is outstanding
Supernatant liquid viscosity is 3310 mPa.s, reaches 6.47 times of raw ore suspension viscosity (512 mPa.s).
Embodiment 4
By attapulgite raw ore by it is broken, to roller extrusion process after, take 1kg to be distributed to the phosphorus of 10kg mass concentration 2%
The suspension that concentration is 10% is made in sour two aqueous ammonium of hydrogen, is then transferred to two sides and is equipped in the container of electrode, at electrode both ends
Apply the alternating current of 220V and 50 Hz, handles 60 min, mechanical stirring disperses 30 min, then applies 1500 V/m of electric field strength
Alternating electric field handles 120 min；Then suspension cyclone classification is removed into quartz sand and large granular impurity, finally carries out filters pressing point
From, dry and pulverization process, the nano-attapulgite stone of high degree of dispersion is obtained.Gained nano-attapulgite stone is distributed in water with 20%
When, concave convex rod stone grain diameter D90≤1.4 micron in suspension, attapulgite stick crystalline substance draw ratio >=30.Nano-attapulgite stone 7%
Water slurry viscosity is 3140 mPa.s, reaches 6.13 times of raw ore suspension viscosity (512 mPa.s).
Embodiment 5
By attapulgite raw ore by it is broken, to roller extrusion process after, take 1kg to be distributed to 20 kg mass, 0.1% di(2-ethylhexyl)phosphate
The suspension that concentration is 5% is made in hydrogen aqueous ammonium, is then transferred to two sides equipped in the container of electrode, applies at electrode both ends
The alternating current of 110V and 1000 Hz handle 60 min, and mechanical stirring disperses 30 min, then apply 1000 V/m of electric field strength friendship
Changed electric field handles 120 min, and suspension cyclone classification is then removed quartz sand and large granular impurity, finally carries out filters pressing point
From, dry and pulverization process, the nano-attapulgite stone of high degree of dispersion is obtained.Gained nano-attapulgite stone is distributed in water with 20%
When, concave convex rod stone grain diameter D90≤0.96 micron in suspension, attapulgite stick crystalline substance draw ratio >=31.Nano-attapulgite stone 7%
Water slurry viscosity is 3360 mPa.s, reaches 6.56 times of raw ore suspension viscosity (512 mPa.s).
Claims (5)
1. a kind of method of alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju, is by attapulgite raw ore by broken, right
After roller extrusion process, it is distributed to and the suspension that mass concentration is 5 ~ 20% is made in the aqueous solution containing chemical assistant, be then transferred to two
Side is equipped in the slot type receptacles of electrode, and applies alternating current at electrode both ends, handles 10 ~ 60 min, then mechanical stirring is dispersed
25 ~ 30 min, then apply alternating electric field and handle 30 ~ 120 min；Then suspension cyclone classification is removed into quartz sand and bulky grain
Impurity most obtains the nano-attapulgite stone of high degree of dispersion through separation, drying, crushing afterwards；The chemical assistant is glycine, third
One of propylhomoserin, diammonium hydrogen phosphate, ammonium dihydrogen phosphate and ammonium phosphate.
2. the method for alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju according to claim 1 a kind of, feature exist
In: the attapulgite purity is greater than 85%.
3. the method for alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju according to claim 1 a kind of, feature exist
In: the voltage of the alternating current is 100 ~ 380 V, and frequency is 50 ~ 1200Hz.
4. the method for alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju according to claim 1 a kind of, feature exist
In: the alternating electric field intensity is 500 ~ 2000 V/m.
5. the method for alternating electric field induction Features of Attapulgite Minerals crystalline substance Shu Xieju according to claim 1 a kind of, feature exist
In: the mass concentration of chemical assistant aqueous solution is 0.1 ~ 2.5%.
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| CN110564487B (en) * | 2019-08-29 | 2021-09-28 | 杭州电子科技大学 | Method for preparing green nano cutting fluid by combining cycloidal ultrasonic stirring with alternating electric field |
| CN113333735A (en) * | 2021-05-07 | 2021-09-03 | 东南大学 | Method for purifying silver nanoparticles by circularly inducing morphology transformation through alternating electric field |
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| CN101898765B (en) * | 2010-07-30 | 2012-05-09 | 淮阴工学院 | Method for effectively dispersing depolymerization and preventing secondary agglomeration of attapulgite clay crystal bundle |
| CN103253654A (en) * | 2012-02-20 | 2013-08-21 | 海洋王照明科技股份有限公司 | Method for preparing graphene by peeling intercalated graphite through electric field |
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