CN100500563C - Method for purifying superfine montmorillonite - Google Patents
Method for purifying superfine montmorillonite Download PDFInfo
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- CN100500563C CN100500563C CNB200710067840XA CN200710067840A CN100500563C CN 100500563 C CN100500563 C CN 100500563C CN B200710067840X A CNB200710067840X A CN B200710067840XA CN 200710067840 A CN200710067840 A CN 200710067840A CN 100500563 C CN100500563 C CN 100500563C
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Abstract
This invention discloses a method for finely purifying montmorillonite. The method comprises: mixing bentonite ore and water at a ratio of 1:(2-9) to obtain slurry, soaking and stirring in a stirrer, sieving with 100-325 mesh sieve to remove large particles, sending the slurry to an ultrafine exfoliation apparatus for ultrafine exfoliation, classifying by a classifier to remove fine sand and obtain ultrapure and ultrafine slurry, dehydrating, drying, and pulverizing to obtain ultrapure and ultrafine montmorillonite. Ultrafine exfoliation effectively breaks the aggregation of montmorillonite and impurity ore, thus can improve the dispersion and suspension performance of montmorillonite, and is advantageous for following classification and purification. Classification by using specific gravity can obtain ultrapure and ultrafine montmorillonite. The method has such advantages as no need for dispersant, simple process, and high yield, and is suitable for mass production.
Description
Technical field
The present invention relates to a kind of method for purifying superfine montmorillonite, belong to the deep process technology field of montmorillonite.
Background technology
Montmorillonite (montmorillonite) has another name called montmorillonite, is the silicate clay ore deposit of a kind of laminate structure, plate crystal, and the city names because of its illiteracy that is found in France is at first taken off, and forms by natural volcanic ash is rotten in geological age.The montmorillonite particle is tiny, about 0.2-1 micron, and tool colloid dispersing characteristic is bulk or earthy aggregate output usually.Observe under electron microscope, crystal belongs to oblique system, generally is irregular sheet.Color is a white band light gray, is with light blue or light red sometimes, the gloss dimness; Mohs' hardness 2-2.5, proportion 2-2.7.Have very strong adsorptive power and ion-exchange capacity, also have colloidality, plasticity-and the cohesive force of height simultaneously, and water-absorbent is very strong, add water and expand, volume can increase several times to tens times.Montmorillonite is widely used in more than 100 departments in 24 fields such as metallurgy, electromechanics, chemical industry, building, coating, oil, weaving, food, water conservancy, traffic, medicine, papermaking, environment protection, novel material, daily necessities, agricultural and livestock industry because of its distinctive physics-chem characteristic; 300 multiple products are arranged, thereby people are referred to as " omnipotent soil ".
Montmorillonite is the main component of bentonite composition, in the natural wilkinite mainly by mineral compositions such as montmorillonite, quartz, feldspar, calcite, kaolinite and illites, smectite content is high more in wilkinite, and mineral deposit quality and effect are good more, and added value is also high more.Therefore, the preparation of high-purity montmorillonite is a focus in montmorillonite deep processing field always.
Superfine nanoization is the inexorable trend of montmorillonite deep process technology development, along with making rapid progress of scientific technological advance, wilkinite equally must be through after the superfine grinding with most non-metallic minerals, reach its functional effect of the nano level fineness competence exertion of micron order, have that specific surface area is big, surfactivity is high, chemical reaction velocity is fast, a good physical and chemical performance such as suspension and good stability, filler reinforcement performance are good, hiding rare height.And satisfy the service requirements of other field.The granularity of the inorganic nonmetal mineral fillers such as wilkinite that require as the functional fiber filler is D
97≤ 2 μ m, maximum particle diameter≤3 μ m; The superpolymer based composites is used also requires wilkinite product granularity D
50≤ 1 μ m, D
97≤ 5～6 μ m.
The montmorillonite method of purification of bibliographical information mainly contains following 5 kinds at present:
1, utilizes the proportion of montmorillonite and impure mineral and the dry purification technology that particle diameter difference is carried out crushing and classification.Because the mutual parcel of impure mineral and montmorillonite, its proportion is also comparatively close, causes particulate impurity separation difficulty, so this method montmorillonite purity raising is limited, and quality product is not good enough.
2, chemical purification method: United States Patent (USP) 3865240 has been introduced a kind of with the sodium hexametaphosphate solution bentonitic method of purifying, and this method changes the viscosity of bentonite slurry liquid system by adding dispersion agent, and the bigger impure mineral of proportion is precipitated.Though this method has reduced the purity of wilkinite slurry, help contamination precipitation, but can not effectively disperse the montmorillonite that wraps up mutually with impure mineral, thereby cause montmorillonite and impurity coprecipitation to get off, the selected efficient of montmorillonite is low, is difficult to obtain greater than the montmorillonite product more than 90%.Owing to containing the phosphoric acid salt dispersion agent, product restricted its application in addition at aspects such as makeup.
3, centrifugal method of purification: carbonato low-grade bentonite raw ore is broken into the grade of 0-5mm in crusher, sends into then and add water in the rotary gas separator and stir and make suspension.The rotating speed of delivering to then in the precipitate and separate device with 1250r/min stirs 2min, 35% montmorillonite is separated, remaining suspension liquid enters in another rotation separate and subside device, rotating speed with 3000r/min changes 2min, 45% montmorillonite is separated, and remaining suspension enters the dry montmorillonite product that gets in the moisture eliminator.Though this method can obtain purity greater than 90% montmorillonite product, because the wilkinite suspension property is limited, through multiple fractionation, productive rate is very low, causes a large amount of wastes of montmorillonite, and water consumption is consuming time.
4, the centrifugal again method of purification of first sodium: this method is general carries out sodium to wilkinite earlier and handles, and then with the method for centrifugal classification, obtains the higher na-montmorillonite of purity.This method sodium is handled more loaded down with trivial details, and extruding sodium method need wear out and improve the wilkinite dispersing property, and the power consumption of solution sodium method water consumption, the wilkinite dispersiveness after the processing improves limited.
Summary of the invention
The object of the invention is to provide that a kind of technology is simple, production efficiency is high, production cost is low, good product performance, is easy to realize the method for purifying superfine montmorillonite of scale operation.
The present invention is a kind of method for purifying superfine montmorillonite, it is characterized in that wilkinite raw ore and water are mixed with slurries by the concentration of weight ratio 1:2～9 of wilkinite raw ore and water, in whipping device, cross 100～325 mesh sieves after the soaking and stirring slurrying and remove large granular impurity, then slurries inputs is delaminated and carry out ultra-fine delaminating in machine, ball mill, stirring mill or the sand mill, the classified sizing of equipment of slurries after ultra-fine the delaminating is removed fine sand and is got the high pure and ultra-fine slurries, and dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last; Slurries size-grade distribution after described ultra-fine the delaminating is: D
50≤ 1.5 μ m, D
75≤ 2 μ m.
The slurrying concentration of described wilkinite raw ore and water can be 1:3～6 by the weight ratio of wilkinite raw ore and water.
Described whipping device can be high speed agitator or changes pulp grinder etc.
Describedly in the machine of delaminating, ball mill, stirring mill or sand mill, carry out the ultra-fine medium of delaminating of delaminating and can be the Ceramic Balls of proportion between 2.5～5.5.
Described stage equipment can be whizzer or hydrocyclone etc.
The size-grade distribution of the high pure and ultra-fine slurries behind the described classified sizing of equipment can be: D
90≤ 2 μ m.
The principle of the method for the invention is:
The natural particle diameter of montmorillonite is minimum, mainly be present in＜2 μ m in, thereby has a bigger surface energy, generally all be gathered into bigger particle, the particle diameter of impure mineral mainly is distributed in the scope greater than 2 μ m, the montmorillonite lamella of reuniting often wraps up mutually with impure mineral such as quartz, be difficult to spread out, so the key that montmorillonite is purified is exactly how to strengthen the dispersed suspension property of montmorillonite.The present invention carries out ultra-fine delaminating by the mode that machinery is delaminated with montmorillonite, thereby the montmorillonite particle of agglomerated separately.Because the hardness ratio impure mineral of montmorillonite is low, therefore in the process of delaminating, the particle diameter of impure mineral changes limited, and delaminate back montmorillonite and impure mineral particle size differences are remarkable.According to Stokes'formula, spheroid square being directly proportional of lowering speed and its radius in solution, add that impure mineral proportion is bigger than montmorillonite,, just can remove impure mineral with the gravity classification method and obtain the high pure and ultra-fine montmorillonite so they have the settling velocity than big difference in water.
The present invention compared with prior art has following outstanding advantage and positively effect:
1, delaminates by ultra-fine, effectively opened the reunion parcel of montmorillonite and impure mineral, improved the dispersion suspension performance of montmorillonite, help further classification and purify; Utilize its difference of specific gravity to carry out classification simultaneously, thereby obtain the high pure and ultra-fine montmorillonite.Ultra-fine high-purity montmorillonite by the method for the invention preparation disperses particle diameter little, and specific surface area is big, high adsorption capacity.
2, method of the present invention does not need raw material is carried out pre-treatment, need not add chemical reagent such as dispersion agent, and it is residual that product does not have reagent, and green natural is more suitable for the raw materials requirement of high-end products such as medicine, makeup, and range of application is wider.
3, method of the present invention is with the ultra-fine of montmorillonite and the combination of purifying, and process is simple, compares the productive rate height with traditional wet purification process, and cost is low, is easy to realize industrialization.
Description of drawings
Fig. 1 is the XRD diffracting spectrum of embodiment 1 described Zhejiang bentonite material;
Fig. 2 is the XRD diffracting spectrum after the ultra-fine purification of embodiment 1 described Zhejiang wilkinite;
Fig. 3 is the XRD diffracting spectrum of embodiment 2 described Sichuan wilkinite raw ores 1;
Fig. 4 is the XRD diffracting spectrum after the embodiment 2 described Sichuan wilkinite raw ore 1 ultra-fine purifications;
Fig. 5 is the XRD diffracting spectrum of embodiment 3 described Sichuan wilkinite raw ores 2;
Fig. 6 is the XRD diffracting spectrum after the embodiment 3 described Sichuan wilkinite raw ore 2 ultra-fine purifications;
Fig. 7 is the XRD diffracting spectrum of embodiment 4 described Henan wilkinite raw ores;
Fig. 8 is the XRD diffracting spectrum after the ultra-fine purification of embodiment 4 described Henan wilkinite raw ores.
Embodiment
Embodiment 1:
With the Zhejiang wilkinite, mainly by mineral compositions such as montmorillonite, quartz, feldspar, kaolin, wherein smectite content is 74%, its XRD diffracting spectrum is seen accompanying drawing 1, press Tu Shui and in homogenizer, cross 200 mesh sieves after the soaking and stirring slurrying, remove large granular impurity, then slurries are imported the MBP80 type and delaminated and carry out ultra-fine delaminating in the machine than (weight ratio of wilkinite raw ore and water) 1:4, delaminating, selected grinding medium proportion is 2.7 in the machine, ultra-fine rear slurry size-grade distribution D
50Be 1.26 μ m, D
75Be 1.98 μ m, fine sand is removed in the swirling flow classification in hydrocyclone of the slurries after ultra-fine, the high-purity slurries size-grade distribution D that obtains after the classification
90Be 1.9 μ m, dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last, and its XRD diffracting spectrum is seen accompanying drawing 2.
From accompanying drawing 2 as can be seen this high pure and ultra-fine montmorillonite meet state-promulgated pharmacopoeia to the loose XRD figure spectrum test regulation of raw material of montmorillonite, content measuring shows that smectite content reaches 95%.
Embodiment 2:
With Sichuan wilkinite raw ore 1, mainly by montmorillonite and quartzy two kinds of mineral compositions, wherein smectite content is 81%, its XRD diffracting spectrum is seen accompanying drawing 3, press Tu Shui and in changing pulp grinder, cross 100 mesh sieves after the slurrying, remove large granular impurity, slurries are imported carried out ultra-fine delaminating in the sand mill then than 1:6, selected grinding medium proportion is 3.2 in the sand mill, ultra-fine rear slurry size-grade distribution D
50Be 1.02 μ m, D
75Be 1.94 μ m, the centrifugal classification in whizzer of the slurries after ultra-fine is removed fine sand, the high-purity slurries size-grade distribution D that obtains after the classification
90Be 1.98 μ m, dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last, and its XRD diffracting spectrum is seen accompanying drawing 4.
From accompanying drawing 4 as can be seen this high pure and ultra-fine montmorillonite meet state-promulgated pharmacopoeia to the loose XRD figure spectrum test regulation of raw material of montmorillonite, content measuring shows that smectite content reaches 97%.
Embodiment 3:
With Sichuan wilkinite raw ore 2, mainly by montmorillonite and quartzy two kinds of mineral compositions, wherein smectite content is 92%, its XRD diffracting spectrum is seen accompanying drawing 5, press Tu Shui and in changing pulp grinder, cross 180 mesh sieves after the slurrying, remove large granular impurity, then slurries are imported the MBP80 type and delaminated and carry out ultra-fine delaminating in the machine than 1:8, delaminating, selected grinding medium proportion is 4.2 in the machine, ultra-fine rear slurry size-grade distribution D
50Be 1.44 μ m, D
75Be 1.73 μ m, the centrifugal classification in whizzer of the slurries after ultra-fine is removed fine sand, the high-purity slurries size-grade distribution D that obtains after the classification
90Be 1.51 μ m, dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last, and its XRD diffracting spectrum is seen accompanying drawing 6.
From accompanying drawing 6 as can be seen this high pure and ultra-fine montmorillonite meet state-promulgated pharmacopoeia to the loose XRD figure spectrum test regulation of raw material of montmorillonite, content measuring shows that smectite content reaches 98%.
Embodiment 4:
With Henan wilkinite raw ore, mainly by mineral compositions such as montmorillonite, feldspar, quartz, vermiculite, cristobalites, wherein smectite content is 65%, its XRD diffracting spectrum is seen accompanying drawing 7, press Tu Shui and in homogenizer, cross 325 mesh sieves after the soaking and stirring slurrying, remove large granular impurity, the slurries input is stirred in the mill carry out ultra-fine delaminating then than 1:2, selected grinding medium proportion is 5.0 in the stirring mill, ultra-fine rear slurry size-grade distribution D
50Be 1.38 μ m, D
75Be 1.86 μ m, the centrifugal classification in whizzer of the slurries after ultra-fine is removed fine sand, the high-purity slurries size-grade distribution D that obtains after the classification
90Be 1.82 μ m, dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last, and its XRD diffracting spectrum is seen accompanying drawing 8.
From accompanying drawing 8 as can be seen this high pure and ultra-fine montmorillonite meet state-promulgated pharmacopoeia to the loose XRD figure spectrum test regulation of raw material of montmorillonite, content measuring shows that smectite content reaches 97%.
Claims (6)
1, a kind of method for purifying superfine montmorillonite, it is characterized in that wilkinite raw ore and water are mixed with slurries by the concentration of weight ratio 1:2～9 of wilkinite raw ore and water, in whipping device, cross 100～325 mesh sieves after the soaking and stirring slurrying and remove large granular impurity, then slurries inputs is delaminated and carry out ultra-fine delaminating in machine, ball mill, stirring mill or the sand mill, the classified sizing of equipment of slurries after ultra-fine the delaminating is removed fine sand and is got the high pure and ultra-fine slurries, and dehydration, drying and crushing get the high pure and ultra-fine montmorillonite at last; Slurries size-grade distribution after described ultra-fine the delaminating is: D
50≤ 1.5 μ m, D
75≤ 2 μ m.
2, by the described a kind of method for purifying superfine montmorillonite of claim 1, it is characterized in that the slurrying concentration of described wilkinite raw ore and water, be 1:3～6 by the weight ratio of wilkinite raw ore and water.
3,, it is characterized in that described whipping device is high speed agitator or changes pulp grinder by the described a kind of method for purifying superfine montmorillonite of claim 1.
4,, it is characterized in that described to carry out the ultra-fine medium of delaminating of delaminating in the machine of delaminating, ball mill, stirring mill or sand mill be the Ceramic Balls of proportion between 2.5～5.5 by the described a kind of method for purifying superfine montmorillonite of claim 1.
5, by the described a kind of method for purifying superfine montmorillonite of claim 1, it is characterized in that described stage equipment is whizzer or hydrocyclone.
6,, it is characterized in that the size-grade distribution of the high pure and ultra-fine slurries behind the described classified sizing of equipment is: D by the described a kind of method for purifying superfine montmorillonite of claim 1
90≤ 2 μ m.
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2364211B1 (en) | 2010-02-16 | 2012-08-10 | Nanobiomatters Industries, S.L. | PROCEDURE FOR OBTAINING LAMINARY PHILOSILICATE PARTICLES WITH CONTROLLED SIZE AND PRODUCTS OBTAINED BY SUCH PROCESS. |
| CN101844772B (en) * | 2010-05-28 | 2012-02-29 | 四川思迈特药业科技有限公司 | Process for purifying montmorillonite |
| CN102951651A (en) * | 2011-08-25 | 2013-03-06 | 金基焕 | Preparation technology of high-purity fine white montmorillonite |
| CN102513201B (en) * | 2011-12-19 | 2014-07-30 | 浙江三鼎科技有限公司 | Preparation method of montmorillonite superfine powder |
| CN102602949A (en) * | 2012-03-03 | 2012-07-25 | 济南康众医药科技开发有限公司 | Preparation method of mineral-fiber-free montmorillonite |
| CN102590019B (en) * | 2012-03-06 | 2014-02-12 | 济南康众医药科技开发有限公司 | Method for measuring montmorillonite and foreign matters of montmorillonite |
| CN102688803A (en) * | 2012-06-15 | 2012-09-26 | 中国矿业大学(北京) | Laminar flow centrifuge beneficiation method of bentonite ore |
| CN103073010B (en) * | 2013-02-04 | 2015-03-04 | 乔敏 | Environment-friendly production process for high-purity montmorillonite |
| CN105016352B (en) * | 2015-08-14 | 2018-05-22 | 安吉高纯蒙脱石有限公司 | A kind of food-grade montmorillonite and its preparation process |
| CN108178160A (en) * | 2018-01-22 | 2018-06-19 | 建昌县建元澎润土有限责任公司 | A kind of method for montmorillonite powder of being delaminated using bentonite preparation |
| CN108405204A (en) * | 2018-03-19 | 2018-08-17 | 田东昊润新材料科技有限公司 | A kind of New type cyclone group production technology suitable for high-purity montmorillonite industrialization processing |
| CN109665535A (en) * | 2019-01-01 | 2019-04-23 | 中国人民解放军63653部队 | One kind being directed to the bentonitic method of purification of middle-low grade |
| CN111795875A (en) * | 2019-04-08 | 2020-10-20 | 南京工业大学 | Preparation method of soil colloid particles |
| CN110743510B (en) * | 2019-09-30 | 2022-06-24 | 浙江长安仁恒科技股份有限公司 | Anion adsorbent and preparation method thereof |
| CN112794336A (en) * | 2021-01-29 | 2021-05-14 | 海南海力制药有限公司 | Purification method of montmorillonite, montmorillonite powder and preparation method thereof |
| CN113013548A (en) * | 2021-02-26 | 2021-06-22 | 武汉理工大学 | Montmorillonite modified lithium battery diaphragm and preparation method thereof |
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