CN100463853C - Method for preparing high-purity montmorillonite - Google Patents
Method for preparing high-purity montmorillonite Download PDFInfo
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- CN100463853C CN100463853C CNB2005101205885A CN200510120588A CN100463853C CN 100463853 C CN100463853 C CN 100463853C CN B2005101205885 A CNB2005101205885 A CN B2005101205885A CN 200510120588 A CN200510120588 A CN 200510120588A CN 100463853 C CN100463853 C CN 100463853C
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Abstract
The invention relates to a process for preparing high-purity montmorillonite, which consists of mixing alta-mud powder, sodium salt powder, and urea powder homogeneously, charging water into dispersible alta-mud, stirring for pulping, and carrying out centrifugal classification. The weight ratio of alta-mud powder, sodium salt powder and urea powder is 1:0.02-0.1:0.03-0.2.
Description
Technical field
The present invention relates to the preparation method 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.The montmorillonite composition be (Na, Ca)
0.33(Al, Mg)
2[Si
4O
10] (OH)
2NH
2O, the content of water is very big.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, tap density is 1-1.1g/mL.Have very strong adsorptive power and ion-exchange capacity.The colloidality, plasticity-and the cohesive force that also have height simultaneously.Water-absorbent is very strong, adds water and expands, and volume can increase several times to tens times, is the main component of bentonite composition.Can be used as drilling mud, the tackiness agent of casting mold sand and iron ore pellets, the weighting agent of papermaking, rubber, makeup does in weaving and the petroleum industry that absorption agent, oil decolour and the raw material of cracking catalyst.
Mainly by mineral compositions such as montmorillonite, quartz, feldspar, calcite, kaolinite and illites, smectite content is high more in the natural wilkinite, and the mineral deposit quality is good more, and effect is good more.Therefore, the preparation of high-purity montmorillonite is a focus in montmorillonite deep processing field always.Early stage high purity montmorillonite product is mainly used in the montmorillonite siccative, common recognition by world's environmental protection siccative industry, all smectite contents just can be described as the montmorillonite siccative at the siccative more than 80%, and the montmorillonite desiccant product mainly is outlet and is used for exported product.Over past ten years, high-purity montmorillonite has had widely to be used, as organic montmorillonite, medicinal smectite, used for cosmetic montmorillonite, inorganic gel with montmorillonite etc.In the organic montmorillonite, smectite content about 90%; Smectite content about 95% in the medicinal smectite; The used for cosmetic montmorillonite, smectite content about 95%; The inorganic gel montmorillonite, smectite content about 88%.Be badly in need of a kind of more highly purified montmorillonite product in the market.
Make a general survey of present bibliographical information, the montmorillonite method of purification mainly contains following several:
1, dry purification: its basic craft course is: raw ore → picking → fragmentation → drying (natural air drying) → grinding → gather dust → classification → packing.Yet because the proportion of impurity and montmorillonite is close, cause particulate impurity separation difficulty, cause this method montmorillonite purity raising limited, this method generally is used for purity greater than 80% and the less demanding montmorillonite of montmorillonite product purity ore deposit purified.
2, chemical purification method: United States Patent (USP) 3865240 has been introduced and has a kind ofly been got method with sodium hexametaphosphate solution purification wilkinite, its method is that the input of wilkinite ore pulp is contained in the dilute solution of industrial Sodium hexametaphosphate 99, make mixture precipitation for a moment, separated again, filter (or centrifugal), drying is made the powdery wilkinite.Though this method has reduced the viscosity of wilkinite slurry, help contamination precipitation, but can not open the distinctive worker's shape of montmorillonite structure makes the impurity that is mixed in wherein separate with montmorillonite, 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 phosphate anion, 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 advances as the dry montmorillonite product that gets in the moisture eliminator.Though this method can obtain purity greater than 90% montmorillonite product, the very low a large amount of wastes that cause montmorillonite of productive rate, water consumption is consuming time, and this method restricted application, only is applicable to the purification of part former state dispersiveness with regard to preferable bentonite ore.
4, the centrifugal again method of purification of first sodium: general pair roller extruding and the solution sodium method of adopting earlier of this method carried out the sodium processing to wilkinite, so that open bentonitic worker's shape structure impure mineral is come out, and the suspension property of enhancing montmorillonite, and then, obtain the higher na-montmorillonite of purity with the method for centrifugal classification.This method sodium is handled more loaded down with trivial details, and extrusion process need wear out and improve the wilkinite dispersing property, and the power consumption of solution sodium method water consumption, the dispersed raising of the wilkinite after the processing is limited.
In sum, the principal element that restricts the wilkinite wet purification at present is how to open bentonitic worker's shape structure, strengthens bentonitic dispersion suspension problem.
Summary of the invention
Technical problem to be solved by this invention is: a kind of preparation method of high-purity montmorillonite is provided, and this method can improve bentonitic dispersion suspension performance, opens bentonitic worker's shape structure impurity is come out, and utilize the gravity classification effect with Impurity removal.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
A kind of preparation method of high-purity montmorillonite, it comprises:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is the above dispersed bentonitic step of 50ml/g;
Dispersed wilkinite is added the water stirring pulping, and centrifugal classification obtains the step of high-purity montmorillonite slurries;
In the above-mentioned steps, the weight ratio of wilkinite powder, sodium salt powder, urea powder is: 1:0.02-0.1:0.03-0.2.
Regulate the high-purity montmorillonite slurries with acid, make pH value 2-4;
Add the V-Brite B deironing;
Add polyacrylamide flocculation dewatering, washing, oven dry, pulverize the high-purity montmorillonite powder.
In the such scheme, wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is specially for the above dispersed bentonitic step of 50ml/g:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed;
Insert in the well heater, be warming up to 60-130 ℃, constant temperature 0.5-2 hour, promptly obtaining expanding doubly was the dispersed wilkinite of 50ml/g.
In the such scheme, wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is specially for the above dispersed bentonitic step of 50ml/g:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed;
Stacked 0.5-3 month, promptly obtaining expanding doubly is the dispersed wilkinite of 50ml/g.
In the such scheme, sodium salt is yellow soda ash or Sodium Fluoride.
The principle of the inventive method is:
The key of wet purification technology is exactly to strengthen bentonitic dispersion suspension performance, opens bentonitic worker's shape structure impurity is come out, and makes full use of wilkinite and impure mineral proportion characteristic, utilizes the gravity classification effect with Impurity removal.
The present invention at first prepares super dispersed wilkinite, has opened bentonitic worker's shape structure and impurity is come out has laid a good foundation for further classification removal of impurities, has also strengthened bentonitic suspension property simultaneously, has improved bentonitic purity and productive rate after the centrifugal classification.
Compared with prior art, the present invention has following outstanding advantage:
1, the synergy by sodium salt and urea, bring out bentonitic performance, particularly made bentonitic dispersiveness and suspension fabulous, helped separating of montmorillonite and other impure mineral, wilkinite is removed with impure mineral when having avoided classification, has improved productive rate and purity.
2, the inventive method is compared with traditional separating and purifying method noted earlier, and productive rate improves 10-25%.
3, owing to added a certain amount of acid, V-Brite B (vat powder) in the product dehydration, removed the impurity in the wilkinite, further and improved product whiteness and purity.
4, it is short that the inventive method also has man-hour, characteristic of low energy consumption.
5, the wilkinite product of purifying through the inventive method foreign ion such as chloride ion-containing, phosphate anion not, applied range.
Description of drawings
Fig. 1 is embodiment 1 an Anji raw ore of calcium base bentonite XRD diffractogram
Fig. 2 is an XRD diffractogram after embodiment 1 Anji calcium-base bentonite is purified
Fig. 3 is embodiment 2 Anji sodium bentonite raw ore XRD diffractograms
Fig. 4 is an XRD diffractogram after embodiment 2 Anji sodium bentonites are purified
Embodiment
The inventive method embodiment 1:
1. raw material: select Anji, Zhejiang light green calcium-base bentonite (Fig. 1) for use, mainly be made up of montmorillonite (M), quartzy (Q), feldspar (F) and kaolinite (K), wherein montmorillonite accounts for 66%, and kaolinite accounts for 6%, and quartz accounts for 21%, and feldspar accounts for 7%.Moisture content about 10%.Original ore powder is broken to 325 orders, whiteness 71%.
2. 100 kilograms of above-mentioned Anji wilkinite powders, 5 kilograms of urea powders and yellow soda ash powder are inserted in the high-speed mixer for 4 kilograms, must expand with 80 ℃ of following mixing 30min of 1000r/min rotating speed doubly is the super dispersed wilkinite of 50ml/g.
3. super dispersed wilkinite is added 900 kg of water stirring pulping.
4. bentonite slurry is got the high-purity montmorillonite slurries through the whizzer centrifugal classification.
5. the high-purity montmorillonite slurries are added the sulphur acid for adjusting pH value to 2-4, add the bleaching of 1 kilogram of vat powder then and remove irony, add at last 0.05 kilogram of flocculation agent polyacrylamide dewater, wash, dry high-purity high galcialite product.
Fig. 2 is the X ray diffracting spectrum of high-purity high galcialite product, compares with X-ray diffraction Fig. 1 of raw ore.The diffraction peak that does not contain any impure mineral among Fig. 2; The theoretical molecular formula of chemical composition analysis and pure montmorillonite is close, therefore can judge that smectite content is greater than 98%.Detect through the whiteness instrument, whiteness is 91.5%.
The inventive method embodiment 2:
1. raw material: select Anji, Zhejiang canescence sodium bentonite raw ore (Fig. 3) for use, mainly be made up of montmorillonite (M), quartzy (Q), feldspar (F) and kaolinite (K), wherein montmorillonite accounts for 77%, and kaolinite accounts for 5%, and quartz accounts for 15%, and feldspar accounts for 3%.Moisture content about 10%.Original ore powder is broken to 325 orders, whiteness 79%.
2. 100 kilograms of wilkinite powders, 5 kilograms of urea powders and 4 kilograms of yellow soda ash powders is evenly mixed, place baking oven, 70 ℃ down baking 180min must to expand doubly be the super dispersed wilkinite of 95ml/g.
3. super dispersed wilkinite is added the water stirring pulping by Tu Shui than 800 kilograms.
4. bentonite slurry is got the high-purity montmorillonite slurries through the whizzer centrifugal classification.
5. high-purity slurries are added the sulphur acid for adjusting pH value to 2-4, add the bleaching of 0.5 kilogram of vat powder then and remove irony and pollute, add at last 0.05 kilogram of flocculation agent polyacrylamide dewater, wash, dry high-purity high galcialite product.
Fig. 4 is the X ray diffracting spectrum of high-purity montmorillonite product, compares with X-ray diffraction Fig. 3 of raw ore.The diffraction peak that does not contain any impure mineral among Fig. 4, the theoretical molecular formula of chemical composition analysis and pure montmorillonite is close, therefore can judge that smectite content is greater than 98%.Detect through the whiteness instrument, whiteness is 93.8%.
The inventive method embodiment 3:
1. bentonite in powder is broken to 325 orders.
2. with 10 kilograms of 100 kilograms of wilkinite powders, 3 kilograms of urea powders and Sodium Fluoride powders, place baking oven, 130 ℃ down baking 180min must to expand doubly be the super dispersed wilkinite of 60ml/g.
Other step is with embodiment 2.
The inventive method embodiment 4:
1. bentonite in powder is broken to 325 orders.
2. with 2 kilograms of 100 kilograms of wilkinite powders, 20 kilograms of urea powders and sodium hydroxide powders, placed outdoor stacking 0.5-3 month, must expand doubly is the super dispersed wilkinite of 95ml/g.
Other step is with embodiment 2.
Claims (4)
1. the preparation method of a high-purity montmorillonite, it is characterized in that: it comprises:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is the above dispersed bentonitic step of 50ml/g;
Dispersed wilkinite is added the water stirring pulping, and centrifugal classification obtains the step of high-purity montmorillonite slurries;
In the above-mentioned steps, the weight ratio of wilkinite powder, sodium salt powder, urea powder is: 1:0.02-0.1:0.03-0.2;
Regulate the high-purity montmorillonite slurries with acid, make pH value 2-4;
Add the V-Brite B deironing;
Add polyacrylamide flocculation dewatering, washing, oven dry, pulverize the high-purity montmorillonite powder.
2. the method for claim 1 is characterized in that: wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is specially for the above dispersed bentonitic step of 50ml/g:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed;
Insert in the well heater, be warming up to 60-130 ℃, constant temperature 0.5-2 hour, promptly obtaining expanding doubly was the dispersed wilkinite of 50ml/g.
3. the method for claim 1 is characterized in that: wilkinite powder, sodium salt powder and urea powder is evenly mixed, and making expands doubly is specially for the above dispersed bentonitic step of 50ml/g:
Wilkinite powder, sodium salt powder and urea powder is evenly mixed;
Stacked 0.5-3 month, promptly obtaining expanding doubly is the dispersed wilkinite of 50ml/g.
4. the method for claim 1, it is characterized in that: sodium salt is yellow soda ash or Sodium Fluoride.
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Families Citing this family (10)
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| CN101602509B (en) * | 2008-06-11 | 2013-08-07 | 浙江海力生制药有限公司 | Method for purifying montmorillonite by utilizing electrophoresis and prepared montmorillonite and application thereof |
| 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 |
| CN102898234B (en) * | 2012-10-15 | 2014-08-13 | 中国科学院合肥物质科学研究院 | Slow release urea and preparation method thereof |
| CN103848430B (en) * | 2012-11-29 | 2016-04-06 | 中国地质大学（北京） | A kind of method of separating-purifying montmorillonite from calcium-base bentonite |
| CN103691371B (en) * | 2013-11-29 | 2016-03-16 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of Electrolyte-resistancomposite composite mineral gel |
| CN104478238B (en) * | 2014-12-17 | 2016-08-24 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of bentonite-based mineral gel and preparation method thereof |
| CN108380363B (en) * | 2018-03-19 | 2019-11-08 | 田东昊润新材料科技有限公司 | A kind of high-purity montmorillonite industrialization purification preparation technique |
| CN110663825A (en) * | 2019-11-16 | 2020-01-10 | 哈密市纳嘉工贸有限责任公司 | Method for preparing feed additive by using bentonite |
| CN114853026B (en) * | 2022-03-30 | 2023-08-08 | 哈工大机器人集团(杭州湾)国际创新研究院 | Preparation method of high-performance lithium bentonite |
| CN114837014B (en) * | 2022-03-30 | 2022-12-13 | 哈工大机器人集团(杭州湾)国际创新研究院 | Preparation method of clay compound for carbonless copy paper |
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