CN107043113B - A kind of method of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam - Google Patents
A kind of method of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam Download PDFInfo
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- CN107043113B CN107043113B CN201710435260.5A CN201710435260A CN107043113B CN 107043113 B CN107043113 B CN 107043113B CN 201710435260 A CN201710435260 A CN 201710435260A CN 107043113 B CN107043113 B CN 107043113B
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- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- 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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Abstract
The invention discloses a kind of methods of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam, it is uniformly to mix attapulgite raw ore with aqueous hydrogen peroxide solution after break process, the thin slice of 0.5 ~ 2 mm thickness is formed through roller processing, it is placed in microwave reactor again and carries out microwave, make that oxidation reaction occurs inside mineral aggregates rapidly, organic matter and cement are cleared up；It is then dispersed in and the suspension that mass concentration is 2.5 ~ 20% is made in methanol aqueous solution, suspension is finally subjected to high-pressure homogeneous processing under 5 ~ 80 MPa pressure, it crosses 450 meshes and obtains uniform suspension, solid product is separated, and dry, pulverize, obtain 1-dimention nano attapulgite material, the excellent product performance, good dispersion have application prospect in numerous areas such as high molecular material reinforcement, function carrier, suspension and thickenings.
Description
Technical field
The present invention relates to the methods of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam, belong to nano material preparation and stick
Native Deep processing of minerals and technical field.
Background technique
Due to having compared with high length-diameter ratio feature, monodimension nanometer material can play the work of " reinforcing bar " in the composite
With significantly improving the mechanical performance of material.Especially natural silicate nano material, as inorganic nano reinforced filling application
When, the processing and heat resistance of composite material can also be obviously improved.
Attapulgite is a kind of aqueous rich magnesium of natural 1-dimention nano grade, aluminosilicate clays mineral, crystal habit in rodlike,
With the nano pore and surface silanol group being intertwined, thus excellent colloid, absorption and reinforcing property are shown, fine
The fields such as chemical industry, environmental protection, functional material, catalysis are applied widely.Due to monodimension nano stick crystal structure, attapulgite
Application in terms of high molecular material reinforcement and catalyst carrier receives significant attention, and the dispersibility of attapulgite is to determine it
The key of reinforcement and carrier property.However, Features of Attapulgite Minerals is in geology forming process, due to stick intergranular there are organic matter and
Cement and hydrogen bond or van der Waals interaction cause stick crystalline substance in Bird's Nest dress or the aggregation of bavin stacking, before inabundant depolymerization,
The characteristic of nano material is not had.Therefore, it is basic to be that it is applied in high end materials field for the depolymerization of attapulgite crystalline substance beam
Premise.
Different from traditional mechanical treatment mode, high pressure homogenization technique be one kind can at normal temperature moment to material generate
The processing mode of pressurization-discharge effect has the characteristics that action time is short, high-efficient and safe operation, can be in brilliant beam
Portion forms hole, just as " Micro-bomb ", stick crystalline substance beam and aggregation is dissociated into monodisperse stick crystalline substance, are that one kind can be used for industry
Change the dispersion and dissociation technique of continuous processing.Relatively hold the study found that assembling as caused by stick intergranular hydrogen bond and Van der Waals force
It is easily dissociated by mechanical processing method, but aggregation caused by the cementation of the organic cement of stick intergranular is difficult to pass through mechanical treatment
Method dissociation.So the organic cement for removing stick intergranular before mechanical treatment is the pass realizing stick crystalline substance beam and utmostly dissociating
Key.
Different from traditional conduction and Convective Heating mode, microwave heating is to penetrate into interior of articles by microwave with the light velocity,
It is changed into thermal energy in time to be heated, has the characteristics that high-efficient, speed is fast, low energy consumption.Meanwhile microwave can and hydrogen peroxide
Equal oxidants generate concerted catalysis oxidation, quickly clear up the organic matter inside material.But utilize micro-wave digestion concave convex rod
Stone crystalline substance beam and the intracorporal organic cement of aggregation, and then weaken the interaction of stick intergranular, then in conjunction with HIGH PRESSURE TREATMENT, improve stick
Brilliant depolymerization efficiency has no that pertinent literature is reported, the precedent that also do not apply.
Summary of the invention
It is to utilize the purpose of the present invention is to provide a kind of method of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam
Attapulgite is assembled intracorporal organic matter and cement is cleared up, weakened by the catalytic oxidation of hydrogen peroxide under microwave action
Then brilliant beam and aggregation dissociation are dispersed into a wiener using the cavitation of high-pressure homogeneous generation by the interaction of stick intergranular
Rice material promotes attapulgite in the application performance in the fields such as high molecular material reinforcement, function carrier and thickening suspension.
Specific method of the invention is: being the peroxide that attapulgite raw ore is used to mass concentration 3.1 ~ 8.5% after broken
Changing aqueous solution of hydrogen adjustment makes attapulgite clay raw ore water content to 35 ~ 39%, obtains 0.5 ~ 2 mm using to roller extrusion process
Thick thin slice；This thin slice is placed in microwave reactor again and carries out microwave treatment, makes to aoxidize rapidly inside mineral aggregates
Reaction clears up organic matter and cement to weaken the interaction of stick intergranular；It is then dispersed in the methanol aqueous solution (matter of methanol
Amount percentage is 5 ~ 10%) in the suspension of mass concentration 2.5 ~ 20% is made, suspension is finally subjected to high-pressure homogeneous processing, mistake
450 mesh vibrating screens, solid product is centrifuged, and be dry, pulverize in 60 ~ 100 DEG C of baking ovens, is obtained 1-dimention nano concave convex rod
Stone.
Content of MgO is greater than 10% in the attapulgite.
The power of microwave treatment is 2.5 ~ 10 KW, and the processing time is 5 ~ 30 min；The high-pressure homogeneous pressure is 5 ~ 80
MPa。
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 that attapulgite raw ore and present invention process prepare nano-attapulgite stone
XRD spectrum.It will be seen from figure 1 that mainly having the characteristic peak of attapulgite and quartz in attapulgite clay, by the present invention
After process, there is no significant changes for attapulgite characteristic peak, but the characteristic diffraction peak of quartz almost disappears, and illustrates this hair
Bright technique is not only brilliant without damage attapulgite stick during depolymerization attapulgite crystalline substance beam, but also also removes quartz sand
Impurity.Fig. 2 is the SEM figure that attapulgite raw ore (a) and technique of the present invention prepare nano-attapulgite stone (b).It can be with from Fig. 2
Find out, attapulgite is nano bar-shape structure, but in raw ore attapulgite stick crystalline substance with the aggregation of dense packing and brilliant beam shape
Formula exists, and the nano stick crystal of independent dispersion is not observed.After present invention process is handled, attapulgite crystalline substance beam and aggregation
It disappears, there are the nanometer rods of a large amount of independent dispersions to occur, illustrate that attapulgite crystalline substance beam and aggregation are depolymerizated and are dispersed into monodisperse
Palygorskite nano stick is brilliant.The nano-attapulgite stone stick crystalline substance length obtained by depolymerization is not bright compared with raw ore medium rod crystalline substance length
Aobvious variation.
The present invention has the advantage that compared with the conventional method
1. assembling intracorporal organic substance and cement using microwave catalysis oxidation reaction resolution attapulgite, biography is overcome
System processing method is only capable of dispersing but cannot removing the deficiency of organic cement；
2. microwave and high-pressure homogeneous synergistic effect combine chemical method and physical method advantage, therefore depolymerization is more efficient,
Product dispersibility is more preferable, and quality is stablized, and suspends suitable for exploitation high molecular material reinforcing agent, function carrier and thickening contour additional
It is worth product；
3. preparation process is simple, it is not related to using high temperature, therefore safe operation, process is easily controllable, and low energy consumption；Technique
In solvent can be recycled, three-waste free discharge.
Detailed description of the invention
Fig. 1 is to obtain the XRD spectrum of attapulgite after attapulgite raw ore and present invention process depolymerization.
Fig. 2 is to obtain the SEM picture of attapulgite after attapulgite raw ore and present invention process depolymerization.
Specific embodiment
Below with by specific embodiment to the method for the microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam of the present invention and
Effect is described further.
Embodiment 1
By 50 kg attapulgite raw ores after break process, the aqueous hydrogen peroxide solution (matter of 32 kg is sprayed thereto
Measure concentration 3.1%), then carry out the piece for handling roller to obtain 0.5 mm thickness；This piece is placed in microwave reactor again, in 10KW
5 min of microwave treatment under power makes that oxidation reaction occurs inside mineral aggregates, organic matter and cement is cleared up；Then will
What the mineral after microwave treatment were directly dispersing in 2000kg methanol aqueous solution (mass fraction of methanol be 10%) is made suspension
Liquid；Gained suspension crosses 500 mesh vibrating screens after this suspension to be carried out to high-pressure homogeneous processing under 80 MPa pressure, and solid is produced
Object centrifuge separation, it is dry in 60 DEG C of baking oven, then through pulverization process, obtain 1-dimention nano attapulgite product.
When gained nano-attapulgite stone is distributed in water with 20%, concave convex rod stone grain diameter D90≤1.2 micron in suspension,
Attapulgite stick crystalline substance average aspect ratio >=30.
Embodiment 2
By 50kg attapulgite raw ore after break process, spraying 32kg aqueous hydrogen peroxide solution thereto, (quality is dense
8.5%) degree, carries out the piece for handling roller to obtain 0.5 mm thickness, this piece is placed in microwave reactor, the microwave under 2.5KW power
30 min are handled, makes that oxidation reaction occurs inside mineral aggregates, organic matter and cement is cleared up；By the mine after microwave treatment
Object is directly dispersing in the methanol aqueous solution (mass fraction of methanol is 10%) of 250 kg and suspension is made, then by suspension
It carries out crossing 500 mesh vibrating screens after high-pressure homogeneous processing under 5 MPa pressure, solid product is centrifugated, in 100 DEG C of dryings,
1-dimention nano attapulgite product is obtained through pulverization process again.
When gained nano-attapulgite stone is distributed in water with 20%, concave convex rod stone grain diameter D90≤1.1 micron in suspension,
Attapulgite stick crystalline substance average aspect ratio >=31.
Embodiment 3
By 50kg attapulgite raw ore after break process, the aqueous hydrogen peroxide solution (quality of 32kg is sprayed thereto
Concentration 3.1%), carry out the piece for handling roller to obtain 2 mm thickness；This piece is placed in microwave reactor, the microwave under 10KW power
20 min are handled, makes that oxidation reaction occurs inside mineral aggregates, organic matter and cement is cleared up；By the mine after microwave treatment
Object, which is directly dispersing in the methanol aqueous solution that 500 kg mass fractions are 5%, is made suspension (mass fraction of methanol is 5%), so
500 mesh vibrating screens are crossed after suspension to be carried out to high-pressure homogeneous processing under 20 MPa pressure afterwards, solid product is centrifugated,
80 DEG C of dryings, then 1-dimention nano attapulgite product is obtained through pulverization process.
When gained nano-attapulgite stone is distributed in water with 20%, concave convex rod stone grain diameter D90≤1 micron, recessed in suspension
Convex stick stone stick crystalline substance average aspect ratio >=32.
Embodiment 4
By 50kg attapulgite raw ore after break process, the aqueous hydrogen peroxide solution (matter of 32 kg is sprayed thereto
Measure concentration 5%), then carry out the piece for handling roller to obtain 1 mm thickness.This piece is placed in microwave reactor, it is micro- under 5KW power
Wave handles 15 min, makes that oxidation reaction occurs inside mineral aggregates, organic matter and cement are cleared up；It again will be after microwave treatment
Mineral be directly dispersing in 750kg methanol aqueous solution (mass fraction of methanol be 10%) suspension be made, then by suspension
500 mesh vibrating screens are crossed after carrying out high-pressure homogeneous processing under 10 MPa pressure, solid product is centrifugated, it is dry at 100 DEG C
It is dry, then 1-dimention nano attapulgite product is obtained through pulverization process.
When gained nano-attapulgite stone is distributed in water with 20%, concave convex rod stone grain diameter D90≤0.98 is micro- in suspension
Rice, attapulgite stick crystalline substance average aspect ratio >=32.
Embodiment 5
By 50kg attapulgite raw ore after break process, the aqueous hydrogen peroxide solution (quality of 32kg is sprayed thereto
Concentration 6.1%), carry out the piece for handling roller to obtain 2 mm thickness；This piece is placed in microwave reactor, the microwave under 10KW power
30 min are handled, makes that oxidation reaction occurs inside mineral aggregates, organic matter and cement is cleared up；It again will be after microwave treatment
Mineral are directly dispersing in the methanol aqueous solution (mass fraction of methanol is 8%) of 1000 kg and suspension are made, and then will suspend
After liquid carries out high-pressure homogeneous processing under 40MPa pressure, after crossing 500 mesh vibrating screens, solid product is centrifugated, at 90 DEG C
It is dry, then 1-dimention nano attapulgite product is obtained through pulverization process.
When gained nano-attapulgite stone is distributed in water with 20%, concave convex rod stone grain diameter D90≤0.96 is micro- in suspension
Rice, attapulgite stick crystalline substance average aspect ratio >=33.
Claims (8)
1. a kind of method of microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam is to use attapulgite raw ore after broken
Aqueous hydrogen peroxide solution adjustment makes attapulgite clay raw ore water content to 35 ~ 39%, using 0.5 is obtained to roller extrusion process ~
The thin slice of 2 mm thickness；This thin slice is placed in microwave reactor again and carries out microwave treatment, makes to occur rapidly inside mineral aggregates
Oxidation reaction clears up organic matter and cement to weaken the interaction of stick intergranular；It is then dispersed in methanol aqueous solution and makes
At suspension, suspension is finally subjected to high-pressure homogeneous processing, 450 mesh vibrating screens is crossed, solid product is centrifuged, is done
It is dry, it crushes, obtains 1-dimention nano attapulgite.
2. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: institute
The mass fraction for stating MgO in attapulgite is greater than 10%.
3. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: mistake
The mass concentration for aoxidizing aqueous solution of hydrogen is 3.1 ~ 8.5%.
4. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: institute
The power for stating microwave treatment is 2.5 ~ 10 k W, and the processing time is 5 ~ 30 min.
5. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: first
The mass percent of methanol is 5 ~ 10% in alcohol solution.
6. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: institute
The mass concentration for stating suspension is 2.5 ~ 20%.
7. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: institute
Stating high-pressure homogeneous pressure is 5 ~ 80 MPa.
8. the method for microwave-assisted high-pressure homogeneous depolymerization attapulgite crystalline substance beam according to claim 1, it is characterised in that: institute
Stating drying is carried out in 60 ~ 100 DEG C of baking ovens.
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| CN109021661A (en) * | 2018-06-19 | 2018-12-18 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of formaldehyde solidification functional material and preparation method thereof and application method |
| CN109264733B (en) * | 2018-10-08 | 2020-05-12 | 临澧县众帮化工有限公司 | Method for improving specific surface area of montmorillonite in anhydrous environment |
| CN109498645A (en) * | 2018-11-28 | 2019-03-22 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Charge regulation cooperates with the high-pressure homogeneous method for preparing attapulgite cationic antibacterial agent |
| CN110436471B (en) * | 2019-09-06 | 2022-10-28 | 中国科学院兰州化学物理研究所 | Method for preparing white dimension-mixed nano silicon material by using red attapulgite clay |
| CN110734073B (en) * | 2019-11-28 | 2021-11-19 | 中国科学院兰州化学物理研究所 | Preparation method of gel factor attapulgite assembled inorganic gel with double network structures |
| CN113637459B (en) * | 2021-07-13 | 2022-07-12 | 中南大学 | Preparation method of composite mineral microsphere-based phase-change heat storage material |
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| CN101898765A (en) * | 2010-07-30 | 2010-12-01 | 淮阴工学院 | Method for effectively dispersing depolymerization and preventing secondary agglomeration of attapulgite clay crystal bundle |
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