CN109665535A - One kind being directed to the bentonitic method of purification of middle-low grade - Google Patents
One kind being directed to the bentonitic method of purification of middle-low grade Download PDFInfo
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- CN109665535A CN109665535A CN201910000247.6A CN201910000247A CN109665535A CN 109665535 A CN109665535 A CN 109665535A CN 201910000247 A CN201910000247 A CN 201910000247A CN 109665535 A CN109665535 A CN 109665535A
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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
- C01B33/40—Clays
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- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses one kind to be directed to the bentonitic method of purification of middle-low grade, middle-low grade bentonite ore was smashed and ground into 200 meshes, obtained bentonite powder is mixed with deionized water, by means of the effect of mechanical force, it comes the mineral grain being bonded together in bentonite is fully dispersed, bentonite slurry is prepared, chemical reagent removal partial impurities are added in scattered bentonite slurry and bentonite chats composition granule is made sufficiently to suspend；Physical purification is carried out to the slurries sufficiently to suspend again, extracts upper layer slurries repeatedly；Then the bentonite upper layer slurries of extraction are carried out dehydrating using centrifugal process, are dried, ground to get the higher bentonite concentrate of purity is arrived, the present invention uses HCl and H2O2The carbonate and organic matter in bentonite slurry are removed, and assists with constant temperature oscillation being sufficiently to react, slurries are sufficiently suspended, so that subsequent physical method refining effect is more preferable, improve purification efficiency.
Description
Technical field
The invention belongs to nonmetallic mineral material fields, and in particular to one kind is directed to the bentonitic purification side of middle-low grade
Method.
Background technique
Bentonite is also known as bentonite, amargosite, is a kind of function admirable, and economic value is higher, and application range is wider to glue
Soil resource.Its main mineral constituent is montmorillonite, is mixed with the big impurity of a certain amount of quartz, feldspar isodensity.Bentonite has
Excellent physicochemical properties, such as water swellability, adsorptivity, dispersion suspension, cationic exchangeability, thixotropy, cohesiveness,
Lubricity etc. makes it play a significant role in a department in 24 fields of national economy more than 100, enjoys the reputation of " omnipotent clay ".
The especially high bentonite of smectite content shows excellent performance in industries such as food, medicine.
China's bentonite resource is abundant, ranks the first in the world, but 80% the above are calcium-base bentonite and grade it is lower, cover de-
It is even lower between the content of stone generally only 50%-80%, belong to middle-low grade bentonite ore.This bentonite resource is due to containing
There are the non-clay minerals such as a large amount of quartz, feldspar to be difficult to carry out deep processing, it is less in the high added values industrial application such as food, medicine.
Therefore, it to improve bentonite Utilization Rate of Mineral Resources, needs carrying out deep processing progress purification processes.
Bentonitic method of purification is generally divided into physical purification method and chemical purification methods two major classes.Physical purification method
That is purification by mineral method can be divided into picking, selection by winnowing (dry purification) and wet concentration (wet purification) by wherein smectite content difference.
Picking is mainly used for the higher bentonite of raw ore smectite content.Stope by manually by ore bulk it is useless
Stone is picked out.
Selection by winnowing (dry purification) is thinner greater than 80%, granularity suitable for smectite content, and gangue mineral (quartz, feldspar)
The thicker ore of granularity.This method is that impure mineral granularity, hardness and density are all larger in foundation natural montmorillonite, by step by step
Separation sedimentation separates impurity, and obtains the very high bentonite of purity.The method is easy to operate, and treating capacity is big, but because of air pollution
Seriously, it separates and is not thorough for impure mineral is with ultra-fine grade product similar in granularity of montmorillonite, for most domestic
The swelling penus middle-low grade method is simultaneously not suitable for, therefore in the industrial production using seldom.
Wet process is then using water as main media, by imposing various external force (gravity, centrifugal force etc.), using covering in bentonite
The difference of de- stone and impurity density, separates impurity and montmorillonite, reaches refining effect.For smectite content in raw ore
Only in the low-grade bentonite of 30%-80%, or it is not very big bentonite for contained feldspar, quartz granularity, obtains higher
The bentonite or montmorillonite of purity often use wet purification.Wet process is sunk according to the different natures that are divided into of purifying technique process again
Drop method, flocculence, supercentrifugal process and secondary grading method etc..
All there is respective advantage and defects when exclusive use a certain kind method in actual purification process.For example,
Natural sedimentation, it be according to montmorillonite in bentonite as clay mineral partial size generally than detrital minerals such as feldspar, quartz
Partial size it is small therefore principle that sinking speed is slow achievees the purpose that Purification of Bentonite.Equipment needed for the method is simple, at low cost, but heavy
Forming sediment, the time is long, take up a large area, production efficiency is lower, and some of which impurity not can be removed very thoroughly.High speed centrifugation
Method and secondary grading method are to separate bentonite suspension through high-speed rotating sedimentation centrifuge, the clast mine of partition size teacher
Object (feldspar, carbonate etc.) obtains bentonite slurry of the granularity less than 5 μm.Different centrifuge speeds and centrifugation time all can
Influence the quality of final products.The centrifugal process purifying technique period is short, high-efficient, but also improves the cost of purification.
Therefore we can use several method, by the excellent of several method in purification process simultaneously in the different stages
Point, which combines, to be used, and improves purification efficiency.
Summary of the invention
The present invention proposes a kind of method of purification for middle-low grade bentonite ore, by physical dispersion, chemical subtraction and from
So sedimentation purification, centrifugal dehydration combine the progress depth purification of centering low-grade bentonite mine.Purifying technique step is simple, grasps
Make convenient and improve purification efficiency, is the deep processing widening roadbed of the bentonite ore of middle-low grade.
The purpose of the present invention is realized by following technical solution: one kind being directed to the bentonitic method of purification of middle-low grade,
The following steps are included:
S1: dispersion slurrying: middle-low grade bentonite ore was smashed and ground into 200 meshes, by obtained bentonite powder and go from
Sub- water is abundant the mineral grain being bonded together in bentonite by means of the effect of mechanical force with the mixing of 1:5-1:12 ratio
It spreads out, bentonite slurry is prepared；
S2: chemical subtraction: different chemical reagent being successively added into bentonite slurry, and being placed in oscillation in constant temperature oscillator makes swelling
Soil comes into full contact with chemical reagent to react, and removes carbonate and organic matter in component respectively.After reaction terminating, stands clarification and incline
Supernatant is removed, is cleaned repeatedly with deionized water, the sufficiently suspension of bentonite chats composition granule is made to prepare suspension；
S3: natural subsidence purification: the slurries sufficiently to suspend stand 8 h, and the suspension of 10 cm depth of upper layer is drawn with siphon pipe,
After extracting every time, the distilled water of equivalent is added, is stirred for, settles, extracts, it is repeated multiple times, it is being provided until deionized water is added
In sedimentation time, it should until extracting the no longer aobvious muddiness of suspension in the depth bounds of suspension；
S4: centrifugal dehydration: being carried out dehydrating using bentonite upper layer slurries of the centrifugal process to extraction, and drying grinds to get arriving
The higher bentonite concentrate of purity.
Further: smectite content is 30%-80% in the middle-low grade bentonite；
Further: the mechanical stirring equipment is electric mixer or magnetic stirring apparatus, 30 min-1h of mixing time；
Further: chemical reagent described in step S2 is respectively HCl and H2O2, and addition sequence is that HCl is first added, reaction
To without obvious blistering, the carbonate in original soil can be effectively removed.Supernatant is outwelled after standing to supernatant clarification.Again plus water
To former scale, H is added2O2, remove the organic matter in component.
Further: auxiliary described in step S2 is with constant temperature oscillation equipment, and vibration temperature is 30-60 DEG C, time 1-2 h.
Further: centrifuge speed is 800-1200 r/min in step S4, and centrifugation time is 3-8 min.
Compared with prior art, present invention is characterized in that
The present invention is purified and is centrifuged on the basis of summarizing traditional bentonitic method, using physical dispersion, chemical subtraction, physical method
It is dehydrated the process combined, the mesh of purification is reached using the good dispersibility of bentonite and the lesser feature of montmorillonite partial size
's.The present invention uses HCl and H2O2The carbonate and organic matter in bentonite slurry are removed, and assists with constant temperature oscillation being to fill
Divide reaction, slurries are sufficiently suspended, so that subsequent physical method refining effect is more preferable, obtains the higher bentonite essence of purity
Mine.
Method of purification step provided by the invention is simple and convenient to operate and improves purification efficiency, can be in low product
The deep processing widening roadbed of the bentonite ore of position.
Detailed description of the invention
Fig. 1 show bentonite original soil and by purification after sample X-ray diffraction spectrogram (XRD).
Fig. 2 show the infrared spectrogram of bentonite original soil and purification soil.
Preferred forms
Below in conjunction with specific embodiment, the present invention is further explained, and following embodiments is only used for illustrating the present invention, and
Protection scope of the present invention is not restricted by the embodiments, and listed material is consistent with the requirement of material noted earlier.
According to Fig. 1-2, one kind is directed to the bentonitic method of purification of middle-low grade, process flow include: pretreatment of raw material,
Disperse slurrying, chemical method removal of impurities, physical method purification, centrifugal dehydration.Specific steps, which are to crush middle-low grade bentonite ore, grinds
Honed 200 mesh mixes obtained bentonite powder with deionized water, by means of the effect of mechanical force, viscous in bentonite
The mineral grain of knot together is fully dispersed to come, and bentonite slurry is prepared；It is added in scattered bentonite slurry
Chemical reagent removal partial impurities simultaneously make bentonite chats composition granule sufficiently suspend；Physics is carried out to the slurries sufficiently to suspend again to mention
It is pure, upper layer slurries are extracted repeatedly；Then the bentonite upper layer slurries of extraction are carried out dehydrating using centrifugal process, are dried, mill
It is broken to get arrive the higher bentonite concentrate of purity.
Embodiment 1:
S1: 200 meshes will be crossed after bentonite raw ore (smectite content 33%) grinding, obtains the swelling that partial size is 0.075 mm
Native powder；It takes bentonite powder and deionized water to be mixed and made into bentonite slurry by solid-to-liquid ratio 1:12, is stirred with electric mixer
24 h are stood after 30 min, regulation system is 0.001 mol/L HCl system, and stirring makes reaction to without obvious blistering, removes former
Carbonate in mine；
S2: supernatant is outwelled after standing to supernatant clarification；Again former scale is added water to, 1 mLH is added2O2, it is placed in constant temperature vibration
It swings in device, 1 h of constant temperature oscillation, reacts it sufficiently under the conditions of 40 DEG C, removes the organic matter in component；By bentonite slurry
After standing makes 8 h of its natural subsidence, 10 cm or more suspension are extracted with siphonage, add deionized water and extraction repeatedly；
S3: the upper layer suspension centrifuge separation of extraction is taken into lower sediment, centrifuge speed is 1000 r/min, and centrifugation time is
8 min；
S4: lower sediment is obtained into purification soil in 50 DEG C of baking oven dries pulverizings；Smectite content is in bentonite after purification
81%。
Embodiment 2:
S1: 200 meshes will be crossed after bentonite raw ore (smectite content 57%) grinding, obtains the swelling that partial size is 0.075 mm
Native powder；It takes bentonite powder and deionized water to be mixed and made into bentonite slurry by solid-to-liquid ratio 1:12, is stirred with electric mixer
24 h are stood after 30 min, regulation system is 0.001 mol/L HCl system, and stirring makes reaction to without obvious blistering, stands extremely
Supernatant is outwelled after supernatant clarification；
S2: adding water to former scale again, and 1 mLH is added2O2, it is placed in constant temperature oscillator, the constant temperature oscillation 1 under the conditions of 40 DEG C
H reacts it sufficiently, removes the reproducibility group in component.After bentonite slurry standing is made 8 h of its natural subsidence, rainbow is used
Suction method extracts 10 cm or more suspension, adds deionized water and extraction repeatedly；
S3: the upper layer suspension centrifuge separation of extraction is taken into lower sediment, centrifuge speed is 1200 r/min, and centrifugation time is
5 min；
S4: lower sediment is obtained into purification soil in 50 DEG C of baking oven dries pulverizings；Smectite content is in bentonite after purification
98%。
Embodiment 3:
S1: 200 meshes will be crossed after bentonite raw ore (smectite content 57%) grinding, obtains the swelling that partial size is 0.075 mm
Native powder；Bentonite powder and deionized water is taken to be mixed and made into bentonite slurry by solid-to-liquid ratio 1:8, with electric mixer stirring 30
24 h are stood after min, regulation system is 0.001 mol/L HCl system, and stirring makes reaction to without obvious blistering, stands to supernatant
Supernatant is outwelled after liquid clarification；
S2: adding water to former scale again, and 1 mLH is added2O2, it is placed in constant temperature oscillator, the constant temperature oscillation 1 under the conditions of 40 DEG C
H reacts it sufficiently, removes the reproducibility group in component.After bentonite slurry standing is made 8 h of its natural subsidence, rainbow is used
Suction method extracts 10 cm or more suspension, adds deionized water and extraction repeatedly；
S3: the upper layer suspension centrifuge separation of extraction is taken into lower sediment, centrifuge speed is 1000 r/min, and centrifugation time is
5 min；
S4: lower sediment is obtained into purification soil in 50 DEG C of baking oven dries pulverizings；Smectite content is in bentonite after purification
95%。
Embodiment 4:
S1: 200 meshes will be crossed after bentonite raw ore (smectite content 57%) grinding, obtains the swelling that partial size is 0.075 mm
Native powder；It takes bentonite powder and deionized water to be mixed and made into bentonite slurry by solid-to-liquid ratio 1:10, is stirred with electric mixer
24 h are stood after 30 min, regulation system is 0.001 mol/L HCl system, and stirring makes reaction to without obvious blistering, stands extremely
Supernatant is outwelled after supernatant clarification；
S2: adding water to former scale again, and 1mL H is added2O2, it is placed in constant temperature oscillator, the constant temperature oscillation 1 under the conditions of 40 DEG C
H reacts it sufficiently, removes the reproducibility group in component.After bentonite slurry standing is made 8 h of its natural subsidence, rainbow is used
Suction method extracts 10 cm or more suspension, adds deionized water and extraction repeatedly；
S3: the upper layer suspension centrifuge separation of extraction is taken into lower sediment, centrifuge speed is 1000 r/min, and centrifugation time is
8 min；
S4: lower sediment is obtained into purification soil in 50 DEG C of baking oven dries pulverizings；Smectite content is in bentonite after purification
96%。
By embodiment 1-4 comparison obtain, comparison purification front and back sample XRD spectra it can be seen that bentonite pass through from
After the purification of heart method, montmorillonite characteristic diffraction peak peak intensity is obviously reinforced, but peak shape is basically unchanged, and purification front and back is " thin and high ".
The width or peak type of spectral line reflect the degree of order and grain size of crystal structure, illustrate to purify base using the method for the invention
This does not influence montmorillonite granular size.And quartzy peak intensity is obviously reduced after purifying, and the feature of high temperature albite and gypsum is spread out
It penetrates peak to disappear substantially, smectite content improves after illustrating purification, can effectively remove impurity, refining effect is preferable, further right
Intensity than the position of the infrared absorption peak on original soil and purification soil spectrogram, peak shape and peak can be seen that by purification, cover de-
Stone characteristic absorption peak intensity increases, and 798 cm-1The characteristic absorption peak for the quartz that place occurs obviously weakens, and illustrates by purification very
The good quartzy impurity eliminated in bentonite, smectite content significantly improve, and the present invention is summarizing the bentonitic method of tradition
On the basis of, the process combined using physical dispersion, chemical subtraction, physical method purification and centrifugal dehydration is good using bentonite
Dispersibility and montmorillonite partial size lesser feature achieve the purpose that purification.The present invention uses HCl and H2O2Remove bentonite
Carbonate and organic matter in slurries, and assist with constant temperature oscillation being sufficiently to react, slurries are sufficiently suspended, so that
Subsequent physical method refining effect is more preferable, obtains the higher bentonite concentrate of purity.
Method of purification step provided by the invention is simple and convenient to operate and improves purification efficiency, can be in low product
The deep processing widening roadbed of the bentonite ore of position.
In the description of the present invention, the terms "include", "comprise" or its any other variant are intended to nonexcludability
Include so that include a series of elements process, method, article or equipment not only include those elements, but also
Including other elements that are not explicitly listed, or further include for this process, method, article or equipment intrinsic want
Element.In the absence of more restrictions, the element limited by sentence " including a reference structure ", it is not excluded that including institute
State in the process, method, article or equipment of element that there is also other identical elements.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. one kind is directed to the bentonitic method of purification of middle-low grade, it is characterised in that: the following steps are included:
S1: dispersion slurrying: middle-low grade bentonite ore was smashed and ground into 200 meshes, by obtained bentonite powder and go from
Sub- water is abundant the mineral grain being bonded together in bentonite by means of the effect of mechanical force with the mixing of 1:5-1:12 ratio
It spreads out, bentonite slurry is prepared；
S2: chemical subtraction: different chemical reagent being successively added into bentonite slurry, and being placed in oscillation in constant temperature oscillator makes swelling
Soil comes into full contact with chemical reagent to react, and removes carbonate and organic matter in component respectively；After reaction terminating, stands clarification and incline
Supernatant is removed, is cleaned repeatedly with deionized water, the sufficiently suspension of bentonite chats composition granule is made to prepare suspension；
S3: natural subsidence purification: the slurries sufficiently to suspend stand 8 h, and the suspension of 10 cm depth of upper layer is drawn with siphon pipe,
After extracting every time, the distilled water of equivalent is added, is stirred for, settles, extracts, it is repeated multiple times, it is being provided until deionized water is added
In sedimentation time, it should until extracting the no longer aobvious muddiness of suspension in the depth bounds of suspension；
S4: centrifugal dehydration: being carried out dehydrating using bentonite upper layer slurries of the centrifugal process to extraction, and drying grinds to get arriving
The higher bentonite concentrate of purity.
2. according to claim 1 be directed to middle-low grade bentonite purification method, it is characterised in that: the middle-low grade is swollen
Smectite content is 30%-80% in profit soil.
3. according to claim 1 be directed to middle-low grade bentonite purification method, it is characterised in that: the mechanical stirring is set
Standby is electric mixer or magnetic stirring apparatus, 30 min-1h of mixing time.
4. according to claim 1 be directed to middle-low grade bentonite purification method, it is characterised in that: change described in step S2
Learning reagent is respectively HCl and H2O2, and addition sequence is that HCl is first added, reaction can effectively remove original to without obvious blistering
Carbonate in soil；Supernatant is outwelled after standing to supernatant clarification；Again former scale is added water to, H is added2O2, remove in component
Organic matter.
5. according to claim 1 be directed to middle-low grade bentonite purification method, it is characterised in that: auxiliary described in step S2
It helps with constant temperature oscillation equipment, vibration temperature is 30-60 DEG C, time 1-2 h.
6. according to claim 1 be directed to middle-low grade bentonite purification method, it is characterised in that: centrifuge in step S4
Revolving speed is 800-1200 r/min, and centrifugation time is 3-8 min.
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| CN201910000247.6A CN109665535A (en) | 2019-01-01 | 2019-01-01 | One kind being directed to the bentonitic method of purification of middle-low grade |
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| CN201910000247.6A CN109665535A (en) | 2019-01-01 | 2019-01-01 | One kind being directed to the bentonitic method of purification of middle-low grade |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573685A (en) * | 2020-06-03 | 2020-08-25 | 湖南师范大学 | Method for preparing organobentonite from calcium-based bentonite raw soil in efficient and environment-friendly manner |
| CN115246648A (en) * | 2022-01-20 | 2022-10-28 | 重庆三峡学院 | Method for extracting clay minerals from shale |
| CN117446815A (en) * | 2023-11-07 | 2024-01-26 | 佛山市顺德区特普高实业有限公司 | Method for preparing montmorillonite with low ferric oxide content and application thereof |
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| CN101049940A (en) * | 2007-03-29 | 2007-10-10 | 浙江三鼎科技有限公司 | Method for purifying superfine montmorillonite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573685A (en) * | 2020-06-03 | 2020-08-25 | 湖南师范大学 | Method for preparing organobentonite from calcium-based bentonite raw soil in efficient and environment-friendly manner |
| CN115246648A (en) * | 2022-01-20 | 2022-10-28 | 重庆三峡学院 | Method for extracting clay minerals from shale |
| CN117446815A (en) * | 2023-11-07 | 2024-01-26 | 佛山市顺德区特普高实业有限公司 | Method for preparing montmorillonite with low ferric oxide content and application thereof |
| CN117446815B (en) * | 2023-11-07 | 2024-06-04 | 佛山市顺德区特普高实业有限公司 | Method for preparing montmorillonite with low ferric oxide content and application thereof |
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