CN107684896A - It is prepared by the recessed soil of loose structure - Google Patents
It is prepared by the recessed soil of loose structure Download PDFInfo
- Publication number
- CN107684896A CN107684896A CN201610624469.1A CN201610624469A CN107684896A CN 107684896 A CN107684896 A CN 107684896A CN 201610624469 A CN201610624469 A CN 201610624469A CN 107684896 A CN107684896 A CN 107684896A
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- China
- Prior art keywords
- polymer microsphere
- recessed
- recessed soil
- loose structure
- soil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
The invention discloses a kind of recessed native preparation method of loose structure.Methods described is to mix the dissociated recessed native aqueous solution with polymer microsphere emulsion, it is prepared into mixed liquor, pass through centrifugal sedimentation, recessed soil is equably mixed with polymer microsphere and be deposited to centrifugation bottom of the tube, upper water is toppled over into removal, is placed in the baking oven of certain temperature and dries, forms the complex of recessed soil and polymer microsphere, polymer microsphere is got rid of by high temperature sintering or organic solvent extracting again, preparation forms the recessed soil of loose structure.The recessed soil of loose structure prepared by the present invention can be used for the purified treatment of waste water, waste gas.
Description
Technical field
The present invention relates to a kind of recessed native preparation method of loose structure, belong to nonmetallic ore field of deep.
Background technology
Recessed soil has special fibre structure, good colloidal property, higher adsorption capacity and certain plasticity
And cohesive force.But recessed soil is earthy aggregate, constructs for compact block, in adsorption treatment on sewage, exhaust process, exist
It is big absorption resistance, the shortcomings of adsorption effect difference.If recessed native structure can be optimized into design, loose structure is prepared into,
It is beneficial to contaminated waste water, waste gas internally spreads from recessed native surface, and then absorbed, purified.
Liu Zi get over et al. application patent《A kind of preparation method of recessed soil/porous carbon composite material》（Application number：
201310232457.0）In, describe and recessed soil/porous charcoal is made in recessed soil and rice husk mixing, suction filtration, alkali activation, high-temperature calcination
Composite.What it was prepared is porous charcoal and attapulgite composite material, rather than the recessed soil of loose structure.The patent of Cui Qun et al. applications
《Attapulgite lay base composite adsorbent for ammonia adsorption refrigeration and its preparation and application》（Application number：200610088249.8）Utilize carboxymethyl
Cellulose, ammonium oxalate or sesbania powder prepare loose structure adsorbent, still, the pore structure so formed can not as expanding agent
Control.
It can be realized using polymer microsphere template and prepare the recessed soil of loose structure.Polymer microsphere template refers to height
Molecule microballoon mixes with target substance presoma, the methods of by centrifugal sedimentation, gravitational settling, forms polymer microsphere and target
The compound of material, then the methods of by extracting or sintering, polymer microsphere is got rid of, form loose structure target substance.Profit
The recessed native aperture of loose structure prepared with polymer microsphere template is easily controllable, is evenly distributed, and is advantageous to waste water, gives up
The adsorption treatment of gas.
The content of the invention
It is used for the recessed native preparation method of loose structure it is an object of the invention to provide a kind of.
Realize that technical scheme step is as follows；
（1）Recessed soil is subjected to acidifying dissociation, abundant mechanical agitation, ultrasonic disperse, forms the recessed native aqueous solution of micro-nano-scale.
（2）Single dispersing or non-mono-disperse polymer microspheres are prepared or purchase, such as crosslinking or Non-cross-linked polystyrene（PS）It is micro-
Ball, crosslinking or non-crosslinked polymethyl methacrylate（PMMA）Microballoon, and other monomers copolymerization microsphere, are configured to finite concentration
Emulsion.
（3）According to the density and particle diameter of different polymer microspheres, by the recessed native aqueous solution and polymer microsphere emulsion according to not
Homogenous quantities ratio is matched, and abundant ultrasonic disperse, is placed in centrifuge tube.
（4）Centrifuge tube is placed in a centrifuge, controls centrifugal speed and time, by recessed soil and polymer microsphere centrifugal sedimentation
To centrifugation bottom of the tube.Water in centrifuge tube is poured off, recessed soil is placed in baking oven with polymer microsphere and dried.
（5）Polymer microsphere is got rid of by high temperature sintering or organic solvent extracting, preparation forms the recessed soil of loose structure.
Step of the present invention（1）The recessed native size of middle preparation can be hundreds of microns to tens microns.
Step of the present invention（2）In polymer microsphere particle diameter can be hundreds of microns to hundreds of nanometers.
Step of the present invention（3）Concave soil is with polymer microsphere mass ratio 1:0.5 and 1:Between 5.Control recessed soil and high score
The mass ratio of sub- microballoon, help to control recessed native hole.
Step of the present invention（4）Middle centrifuge speed and time with recessed soil and polymer microsphere can Equalsettlement disperse
It is advisable, recessed soil is with the drying temperature of polymer microsphere in an oven at 40-80 DEG C.
Step of the present invention（5）Middle sintering temperature is 350-550 DEG C, and is sintered in the case where being passed through air conditionses, avoids height
Molecule microballoon is sintered into charcoal when completely cutting off air, and can not form pore space structure.Control 350-550 DEG C of mesh in sintering temperature
Be to remove polymer microsphere, while do not destroy the intrinsic crystal structure of recessed soil.Can for noncrosslinking polymer microsphere
It is stripped using organic solvent such as toluene, dimethylbenzene, dimethylformamide etc., is then utilized for noncrosslinking polymer microsphere
Sintering removes polymer microsphere.
Brief description of the drawings
The composite electron microscope picture of recessed soil and polymer microsphere prepared by Fig. 1 present invention.
The recessed native electron microscope picture of loose structure prepared by Fig. 2 present invention.
Embodiment
With reference to specific embodiment, the recessed native preparation method of loose structure is explained.
Embodiment 1
1. weighing the recessed soil of the acidified processing of 2.5g, the 250ml aqueous solution is configured to, using homogenizer with 8000rmp's
Rotating speed stirs 15m minutes, then with supersonic wave cleaning machine ultrasonic disperse 10 minutes.
2. measure particle diameter be 1-5um PS microballoon emulsions, by it is recessed soil with PS microballoons according to mass ratio be 1：4 are matched,
It is encased in 50ml centrifuge tubes, adds deionized water and be diluted to 45ml, ultrasonic disperse.
3. using centrifuge with 3000rmp rotating speed centrifugal sedimentation 15 minutes.Supernatant after centrifugation is gone, residue is solid
Body is placed in 45 DEG C of baking ovens and dried.
Being sintered 4. the solid after drying is placed in the Muffle furnace for blast air, Muffle furnace programming rate is 50 DEG C/h,
350 DEG C are risen to from normal temperature, in 350 DEG C of constant temperature 2 hours.After the completion of sintering, allow Muffle furnace to be down to room temperature naturally, finally take out sintering
Later product.
Embodiment 2
1. weighing the recessed soil of the acidified processing of 2.5g, the 250ml aqueous solution is configured to, using homogenizer with 8000rmp's
Rotating speed stirs 15m minutes, then with supersonic wave cleaning machine ultrasonic disperse 10 minutes.
2. measure particle diameter be 5-10um PMMA microsphere emulsion, by it is recessed soil with PMMA microsphere according to mass ratio be 1：4 are carried out
Proportioning, is encased in 50ml centrifuge tubes, adds deionized water to 45ml, ultrasonic disperse.
3. using centrifuge with 3000rmp rotating speed centrifugal sedimentation 15 minutes.Supernatant after centrifugation is gone, residue is solid
Body is placed in 45 DEG C of baking ovens and dried.
4. the solid after drying is placed in solvent dimethylformamide, place 24 hours.
5. solvent dimethylformamide is toppled over, remaining solid is placed in 45 DEG C of baking ovens and dried.
Claims (9)
1. the recessed native preparation method of loose structure is as follows：
（1）Recessed soil is subjected to acidifying dissociation, abundant mechanical agitation, ultrasonic disperse, forms the recessed native aqueous solution of micro-nano-scale.
2.（2）The recessed native aqueous solution is mixed with polymer microsphere emulsion according to certain mass ratio, abundant ultrasonic disperse.
3.（3）The recessed soil and the emulsion of polymer microsphere of abundant ultrasonic disperse are placed in centrifuge tube, using centrifuge carry out from
The heart settles, and is then poured off the water in centrifuge tube, recessed soil is placed in baking oven with polymer microsphere and dried.
4.（4）Polymer microsphere is got rid of by high temperature sintering or organic solvent extracting, preparation forms the recessed soil of loose structure.
5. recessed soil as claimed in claim 1 is acidified processing, grain size is micro-nano meter ruler after Mechanical Crushing, ultrasonic disperse
The recessed soil of degree.
6. polymer microsphere as claimed in claim 1 is crosslinking or Non-cross-linked polystyrene（PS）Microballoon, crosslinking or non-crosslinked
Polymethyl methacrylate（PMMA）Microballoon, and the polymer microsphere of other monomers copolymerization, its particle size can be according to recessed
Native size is adjusted, and particle diameter distribution can be single dispersing or non-single dispersing.
7. the centrifugal speed of centrifuge as claimed in claim 1 and time are deposited in centrifuge tube bottom according to recessed soil and polymer microsphere
The distribution situation in portion is adjusted.
8. the temperature dried in an oven is advisable for the softening temperature no more than polymer microsphere.
9. sintering temperature as claimed in claim 1 is no more than 550 DEG C, decomposition temperature is sintered not less than polymer microsphere；Take out
Extraction solvent is organic solvent such as toluene, dimethylbenzene, the dimethylformamide etc. that can be swelled polymer microsphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610624469.1A CN107684896A (en) | 2016-08-03 | 2016-08-03 | It is prepared by the recessed soil of loose structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610624469.1A CN107684896A (en) | 2016-08-03 | 2016-08-03 | It is prepared by the recessed soil of loose structure |
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| Publication Number | Publication Date |
|---|---|
| CN107684896A true CN107684896A (en) | 2018-02-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610624469.1A Pending CN107684896A (en) | 2016-08-03 | 2016-08-03 | It is prepared by the recessed soil of loose structure |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101658785A (en) * | 2009-09-08 | 2010-03-03 | 湖南大学 | Preparation method of porous silicate powder capable of adsorbing indoor harmful gases |
| CN104795247A (en) * | 2015-04-28 | 2015-07-22 | 中科院广州化学有限公司南雄材料生产基地 | Polyaniline nano-composite electrode material with porous structure, preparation method of polyaniline nano-composite electrode material and application of polyaniline nano-composite electrode material |
-
2016
- 2016-08-03 CN CN201610624469.1A patent/CN107684896A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101658785A (en) * | 2009-09-08 | 2010-03-03 | 湖南大学 | Preparation method of porous silicate powder capable of adsorbing indoor harmful gases |
| CN104795247A (en) * | 2015-04-28 | 2015-07-22 | 中科院广州化学有限公司南雄材料生产基地 | Polyaniline nano-composite electrode material with porous structure, preparation method of polyaniline nano-composite electrode material and application of polyaniline nano-composite electrode material |
Non-Patent Citations (1)
| Title |
|---|
| 梁卫东等: ""乙烯基三乙氧基硅烷改性凹凸棒土多孔亲油材料的制备及吸附性能"", 《非金属矿》 * |
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Application publication date: 20180213 |