CN101823722A - Method for preparing bentonite inorganic gel from calcium bentonite - Google Patents
Method for preparing bentonite inorganic gel from calcium bentonite Download PDFInfo
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Abstract
The invention discloses a method for preparing bentonite inorganic gel from calcium bentonite. The process of the method comprises the steps of starting with calcium bentonite raw ore and using a wet purification modification synchronization process to carry out sodium modification on the calcium bentonite. The sodium modification reaction can improve the expanding and dispersing capacity of montmorillonite, the montmorillonite is easy to be stripped to be at the colloidal particle level under the action of the added dispersing agent and the stirring force for maintaining slurry suspension so as to be easily separated from the impurity minerals which cannot reach the colloidal particle level, thus, the purity and the whiteness of the purified and modified bentonite can be ensured. The high-purity sodium bentonite slurry obtained by wet purification modification does not need to be dehydrated and dried and is directly used for preparing the bentonite inorganic gel. The montmorillonite layers of the sodium bentonite slurry are dispersed well, thus, the prepared bentonite inorganic gel has stable structure and higher viscosity. Meanwhile, considering different requirements of different industries for the viscosity of the bentonite inorganic gel, the method controls the viscosity and the whiteness of the prepared bentonite inorganic gel by controlling the type and dosage of the gelatinizing agent and different gelatinizing conditions.
Description
Technical field
The present invention relates to a kind of nonmetal wilkinite raw ore deep process technology, refer in particular to the method for preparing bentonite inorganic gel by the natural calcium base bentonite.
Background technology
Wilkinite has performances such as swelling property, cementability, adsorptivity, thixotropy, plasticity-, oilness and cationic exchange preferably, it is one of clay mineral that present range of application is wide, economic worth is higher, be widely used in fields such as metallurgy, machinery, oil, chemical industry, medicine, environmental improvement, be called as " clay " with thousand kinds of purposes.Difference according to the cation type that adsorbs between montmorillonite layer can be divided into wilkinite calcium-base bentonite, sodium bentonite, hydrogen (aluminium) base bentonite, magnesium base bentonite etc.China's wilkinite mineral products aboundresources, widely distributed, total reserves is at the forefront in the world, but 90% is calcium-base bentonite.Because there are birth defects such as water-intake rate is little, expansion multiple is low, cation exchange capacity is little, poor lubricity, poor heat stability in calcium-base bentonite, seldom directly applies in the productive life.Therefore need be processed into usually as wilkinite deep processed products such as particle wilkinite, sodium bentonite, organobentonite, atlapulgite, bentonite gels in actual applications, just can be widely used in each field such as petrochemical complex, grease, medicine, building, daily use chemicals, weaving, coating, metallurgy, environmental protection.
Bentonite inorganic gel is to be the mineral coagulant that raw material prepares through deep processing with the wilkinite, this gel has excellent colloidal property, rheological, ion exchangeable, resistance to acids and bases, adsorptivity etc., all is widely used in industries such as environmental protection, building materials, daily-use chemical industry, papermaking, casting, pharmacy; Especially high purity, high whiteness bentonite inorganic gel have great using value in industries such as medicine, food, makeup.The preparation bentonite gel is the effective way that improves wilkinite using value and economic worth.
Wilkinite is to contain the clay that smectite type mineral is the master, and each wilkinite particle all is made up of thousands of small montmorillonite crystal nano flakes.The montmorillonite crystal is formed by two-layer silicon-oxy tetrahedron therebetween layer of aluminum (magnesium) oxygen (hydrogen-oxygen) is octahedra.Owing to have a spot of silicon to be replaced in the montmorillonite crystal tetrahedron by aluminium, there is a spot of aluminium to be replaced in the octahedron by magnesium, make and produce permanent negative charge between crystal layer, thereby between crystal layer absorption a large amount of tradable positively charged ions, in the time of mineral inorganic gel and water blended, the latter sees through the zone between the small pieces, carries out hydration with these inorganic cations on the montmorillonite sheet surfaces, that be in the charge balance state that associate.The montmorillonite lamella that progressively deeply forces of hydration further separates, and the interchangeability positively charged ion just progressively spreads from the surface of montmorillonite lamella and comes, and fully separates up to the montmorillonite lamella, thereby makes montmorillonite form stable double electrical layers.Because montmorillonite crystal nano flake seamed edge is the band portion positive charge under certain condition, this moment, the small pieces seamed edge just attracted to electronegative die surfaces there, set up three-D space structure (being commonly referred to " card room formula " structure) rapidly, the very fast increase of the viscosity of system.When applying a shearforce, the major part in this structure can be disintegrated rapidly, and when shearforce was removed, this structure formed again, thereby the dispersion liquid of bentonite gel has fabulous thixotropy.
Chinese patent CN1363515A discloses a kind of preparation method of natural magnesium aluminium silicate gel.Comprise in this invention key step that wet method slurrying, viscosity-depression agent dispersion, dynamically centrifugation purification, monovalent metallic ion preactivate are handled, Na
+Modification, aftertreatment etc.Though this invention can realize preparing aluminium magnesium silicate inorganic gel by natural smectite well, but this technology is loaded down with trivial details and energy consumption is too high, and the viscosity of products obtained therefrom relatively low (100-500 milli handkerchief second), can not fine satisfied medicine, the particular requirement in field such as food.
Chinese patent CN1257103C improves the defective of above-mentioned patent, has increased intensity magnetic separator deironing and alcohol agent washing twice step, has improved the whiteness and the purity of product.But this technology still exists, and technology is comparatively loaded down with trivial details, the more high shortcoming of production cost.
Chinese patent CN1286719C is further improved above-mentioned patent, increased in process of production ore pulp has been carried out the ultrasonication step, make mineral in water, further peel off, disperse, (viscosity number was 983 milli handkerchief seconds after a supersound process to have improved physical and chemical performances such as colloid output capacity, fineness, purity, whiteness, it was 1382 milli handkerchief seconds that twice ultrasonic is handled the back viscosity number, and gel purity all reaches 99%), but a large amount of ultrasonication certainly will be brought disadvantageous effect to production technique and production cost in suitability for industrialized production.
With regard to bentonite inorganic gel, the purity of gel, whiteness and viscosity depend primarily on the effect of peeling off of montmorillonite crystal lamella in bentonitic purity and the gel preparation course.If be mixed with the impurity of too many other dissociation in water difference in the wilkinite, then it will inevitably have a strong impact on bentonite gel space " card room formula " stability of structure, and the existence of impurity simultaneously also can influence the whiteness of bentonite gel.Montmorillonite crystal lamella peel off effect with the lamella hydration time energy got involved relevant, because mechanical energy and heat energy all can promote the carrying out of hydration, therefore use high shear mixing or reacting by heating all will reduce hydration time, form more stable " card room formula " structure bentonite inorganic gel, thereby obtain higher viscosity and better thixotropy.Therefore the preparation of high-quality bentonite inorganic gel need be controlled two key points: the one, and smectite content is enough high to guarantee bentonite gel " card room formula " stability of structure in the wilkinite; The 2nd, suitable remodeling agent and modified method are to promote the formation of gel.
Summary of the invention
The technical problem to be solved in the present invention provides and a kind ofly prepares the method for bentonite inorganic gel by calcium-base bentonite, and this preparation method is made up of slurrying, the operations such as remodeling, gel of purifying.With the raw ore of calcium base bentonite is starting point, use wet purification remodeling synchronous process that calcium-base bentonite is carried out sodium modification, guarantee bentonitic purity and whiteness, guarantee the viscosity of gel in conjunction with suitable gel method, and then prepare high purity, high whiteness, High Viscosity Bentonite inorganic gel.
The technical problem to be solved in the present invention is realized by following scheme: will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 10%～30% slurries, stirring and evenly mixing after the immersion disintegration, the dispersion agent that adds wilkinite quality 0.2%～1.0%, stirring and dissolving, dispersion agent is one or both in Sodium hexametaphosphate 99 or the trisodium phosphate, be preferably Sodium hexametaphosphate 99, the saturated aqueous solution that adds the remodeling agent of wilkinite quality 3～8%, stirring makes it thorough mixing, ageing 18-24 hour, the remodeling agent can be sodium hydroxide, Sodium Fluoride, yellow soda ash, Sodium hexametaphosphate 99 or trisodium phosphate, be preferably yellow soda ash, after removing lower floor's large granular impurity, system is heated to 70～90 ℃, violent stirring and moisturizing were in good time fully reacted system 1～2 hour under this temperature, after leaving standstill removal lower floor residue, in high speed dispersor, disperseed 0.5～1 hour, thin up is to 3～4 times of original volume, after leaving standstill 1～1.5 hour, siphon obtains the upper strata ore pulp, discard lower floor's residue, centrifugation, discard the thin slag of lower floor, obtain the sodium bentonite concentrate slurry, control solid content about 4～5%, the peptizing agent that adds wilkinite quality 4%～20%, after gel, obtain bentonite inorganic gel, dry, obtain the bentonite inorganic gel product after the dehydration, peptizing agent can be in calcium oxide or the calcium chloride a kind of, wherein calcium oxide is fit to preparation High Viscosity Bentonite inorganic gel product (range of viscosities: 500～3000 milli handkerchief second), and calcium chloride is fit to the relatively low bentonite inorganic gel product of preparation viscosity (range of viscosities: 100～500 milli handkerchief second).The gel condition can be disperseed (4000～20000 rev/mins were disperseed 1～10 minute) for reacting by heating (70～90 ℃ following stirring reaction 1～2 hour) or at a high speed even matter.
Below be schematic illustration of the present invention: produce permanent negative charge owing to isomorphous substitution between the montmorillonite crystal layer in the wilkinite, thereby between crystal layer, adsorb a large amount of tradable positively charged ions.The technology that the present invention adopts is that wet method remodeling carries out simultaneously with wet purification, and water medium provides space and power for expansion between montmorillonite layer with aquation during wet processes, can easily realize the artificial natridization by ion-exchange.Because sodium ion has stronger hydration than calcium ion, so the montmorillonite expansion dispersive ability that improved of natridization reaction.And at the remodeling dispersion agent that adds and keep under the effect of the whipping force that ore pulp suspends, montmorillonite is easy to be stripped to the micelle level, thereby is easy to separate with the impure mineral that does not reach the micelle level, so can obtain comparatively ideal refining effect.After adding the unnecessary negative charge of peptizing agent equilibrium system in the sodium bentonite ore pulp behind above-mentioned purification remodeling, these abundant dispersive montmorillonite crystal lamellas join at electrostatic interaction lower end-face, form unique " card room formula " structure.Comprise a large amount of irreducible water in this " card room formula " structure, thereby obtain having full-bodied bentonite inorganic gel.
The present invention is starting point with the raw ore of calcium base bentonite, use the synchronous technology of wet purification remodeling that calcium-base bentonite is carried out sodium modification, because the carrying out of natridization reaction can be improved the expansion dispersive ability of montmorillonite, and at the dispersion agent that adds and keep under the effect of the whipping force that ore pulp suspends, montmorillonite is easy to be stripped to the micelle level, thereby be easy to separate with the impure mineral that does not reach the micelle level, remodeling bentonitic purity in back and whiteness therefore can guarantee to purify.High pure sodium base bentonite slurries drying-free behind the wet purification remodeling is directly used in the preparation bentonite inorganic gel, because the dispersion of slurries montmorillonite layer is better, so the bentonite inorganic gel Stability Analysis of Structures of preparation, viscosity is higher.Consider that simultaneously different industries is not quite similar to the requirement of bentonite inorganic gel viscosity, the present invention controls the viscosity of prepared bentonite inorganic gel by type, consumption and the gel method of control peptizing agent.
Advantage of the present invention:
1. adopt wet method that calcium-base bentonite is carried out sodium modification, take the technology of purifying and retrofiting and carrying out simultaneously, purification operations runs through whole flow process, the remodeling back wilkinite that guaranteed to purify has higher purity and whiteness, thereby makes final prepared bentonite inorganic gel have the characteristics of high purity, high whiteness.
2. the high pure sodium base bentonite slurries drying-free behind the wet purification remodeling is directly used in the preparation bentonite inorganic gel, has omitted the dehydration of highly energy-consuming.Because above-mentioned sodium bentonite slurries montmorillonite layer disperses better to need not newly to add dispersion agent, guaranteed that the gel process forms bentonite gel space " card room formula " structure easily, makes gellifying property excellent more.
3. selected peptizing agent is calcium oxide and calcium chloride, and product viscosity can be according to the customer requirements adjustment.Wherein calcium oxide is fit to preparation High Viscosity Bentonite inorganic gel product (range of viscosities: 500～3000 milli handkerchief second), and calcium chloride is fit to the relatively low bentonite inorganic gel product of preparation viscosity (range of viscosities: 100～500 milli handkerchief second).
4. gel condition is available, can be reacting by heating (70～90 ℃ following stirring reaction 1～2 hour), also can spare matter at a high speed and disperse (4000～20000 rev/mins were disperseed 1～10 minute).
5. simple for process, desired raw material (Na
2CO
3, (NaPO
3)
6, CaO etc.) cheaply be easy to get, thereby realize less energy-consumption, low-cost preparation high-quality bentonite inorganic gel.
Description of drawings
Fig. 1 process flow sheet of the present invention
Embodiment
Embodiment 1
(1) will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 20% slurries, soaks stirring and evenly mixing after the disintegration.(2) sodium hexametaphosphate dispersant (NaPO of adding wilkinite quality 1.0%
3)
6, in system, add the remodeling agent yellow soda ash Na of wilkinite quality 4% then
2CO
3Saturated aqueous solution, stir and to make it thorough mixing and ageing 24 hours.(3) 90 ℃ are stirred down fully reaction 1 hour, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 0.5 hour.(4) system is diluted to original volume to 4 times, leave standstill 1.5 hours after, siphon obtains the upper strata ore pulp, discards lower floor's residue.Centrifugation discards the thin slag of lower floor, obtains the sodium bentonite concentrate slurry.(5) evaporation section moisture content is controlled at 5% with the solid content of sodium bentonite concentrate slurry, in the sodium bentonite concentrate slurry, add peptizing agent calcium oxide CaO then, add-on is 8% of a wilkinite quality, obtain bentonite inorganic gel in reaction under 90 ℃ after 1.5 hours, obtain the bentonite inorganic gel product after drying, the dehydration, the viscosity of this bentonite inorganic gel was 1750 milli handkerchief seconds after measured, and whiteness is 85.
Embodiment 2
(1) will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 20% slurries, soaks stirring and evenly mixing after the disintegration.(2) sodium hexametaphosphate dispersant (NaPO of adding wilkinite quality 0.8%
3)
6, in system, add the remodeling agent yellow soda ash Na of wilkinite quality 4% then
2CO
3Saturated aqueous solution, stir and to make it thorough mixing and ageing 20 hours.(3) 85 ℃ of following violent stirring were fully reacted 1 hour, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 0.5 hour.(4) system is diluted to original volume to 4 times, leave standstill 1.5 hours after, siphon obtains the upper strata ore pulp, discards lower floor's residue.Centrifugation discards the thin slag of lower floor, obtains the sodium bentonite concentrate slurry.(5) evaporation section moisture content is controlled at 5% with the solid content of sodium bentonite concentrate slurry, in the sodium bentonite concentrate slurry, add peptizing agent calcium oxide CaO then, add-on is 14% of a wilkinite quality, disperse to obtain in 5 minutes bentonite inorganic gel down at 10000 rev/mins, obtain the bentonite inorganic gel product after drying, the dehydration, the viscosity of this bentonite inorganic gel was 1950 milli handkerchief seconds after measured, and whiteness is 83.
Embodiment 3
(1) will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 20% slurries, soaks stirring and evenly mixing after the disintegration.(2) sodium hexametaphosphate dispersant (NaPO of adding wilkinite quality 1.0%
3)
6, in system, add the remodeling agent yellow soda ash Na of wilkinite quality 4% then
2CO
3Saturated aqueous solution, stir and to make it thorough mixing and ageing 18 hours.(3) 90 ℃ of following violent stirring were fully reacted 1 hour, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 0.5 hour.(4) system is diluted to original volume to 4 times, leave standstill 1.5 hours after, siphon obtains the upper strata ore pulp, discards lower floor's residue.Centrifugation discards the thin slag of lower floor, obtains the sodium bentonite concentrate slurry.(5) evaporation section moisture content is controlled at 5% with the solid content of sodium bentonite concentrate slurry, in the sodium bentonite concentrate slurry, add peptizing agent calcium oxide CaO then, add-on is 12% of a wilkinite quality, disperse to obtain in 5 minutes bentonite inorganic gel down at 6000 rev/mins, obtain the bentonite inorganic gel product after drying, the dehydration, the viscosity of this bentonite inorganic gel was 1650 milli handkerchief seconds after measured, and whiteness is 83.
Embodiment 4
(1) will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 20% slurries, soaks stirring and evenly mixing after the disintegration.(2) sodium hexametaphosphate dispersant (NaPO of adding wilkinite quality 0.8%
3)
6, in system, add the remodeling agent yellow soda ash Na of wilkinite quality 4% then
2CO
3Saturated aqueous solution, stir and to make it thorough mixing and ageing 24 hours.(3) 90 ℃ of following violent stirring were fully reacted 1 hour, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 0.5 hour.(4) system is diluted to original volume to 4 times, leave standstill 1.5 hours after, siphon obtains the upper strata ore pulp, discards lower floor's residue.Centrifugation discards the thin slag of lower floor, obtains the sodium bentonite concentrate slurry.(5) evaporation section water is controlled at 5% with the solid content of sodium bentonite concentrate slurry, adds peptizing agent calcium chloride CaCl then in the sodium bentonite concentrate slurry
2, add-on is 8% of a wilkinite quality, disperses down to obtain in 5 minutes bentonite inorganic gel at 10000 rev/mins, obtains the bentonite inorganic gel product after dry, the dehydration, and the viscosity of this bentonite inorganic gel was 230 milli handkerchief seconds after measured, and whiteness is 88.
Embodiment 5
(1) will adding water less than the raw ore of calcium base bentonite of 1cm through coarse crushing to particle diameter, to be mixed with solid content be 20% slurries, soaks stirring and evenly mixing after the disintegration.(2) sodium hexametaphosphate dispersant (NaPO of adding wilkinite quality 1.0%
3)
6, in system, add the remodeling agent yellow soda ash Na of wilkinite quality 4% then
2CO
3Saturated aqueous solution, stir and to make it thorough mixing and ageing 24 hours.(3) 90 ℃ of following violent stirring were fully reacted 1 hour, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 0.5 hour.(4) system is diluted to original volume to 4 times, leave standstill 1.5 hours after, siphon obtains the upper strata ore pulp, discards lower floor's residue.Centrifugation discards the thin slag of lower floor, obtains the sodium bentonite concentrate slurry.(5) evaporation section moisture content is controlled at 5% with the solid content of sodium bentonite concentrate slurry, adds peptizing agent calcium chloride CaCl then in the sodium bentonite concentrate slurry
2, add-on is 10% of a wilkinite quality, 90 ℃ down reaction obtain bentonite inorganic gel after 1 hour, obtain the bentonite inorganic gel product after dry, the dehydration, the viscosity of this bentonite inorganic gel was 150 milli handkerchief seconds after measured, whiteness is 85.
Claims (3)
1. the preparation method of a bentonite inorganic gel, its process comprise operations such as slurrying, remodeling purification, modification, gel, it is characterized in that the sodium modification of calcium-base bentonite purified disperse with bentonite inorganic gel, the gel process organically combines.High pure sodium base bentonite slurries drying-free behind the wet purification remodeling, be directly used in the preparation bentonite inorganic gel, this process has reduced the dehydration energy consumption on the one hand, on the other hand owing to above-mentioned sodium bentonite slurries polynite purity height, lamella good dispersity, need not newly to add dispersion agent, guaranteed that the gel process forms bentonite gel space " card room formula " structure easily, has improved gellifying property.
2. the preparation method of a kind of bentonite inorganic gel according to claim 1, the amount ranges that it is characterized in that peptizing agent is the 4%-20% of pure soil property amount, when wherein being peptizing agent with the calcium oxide, the 4%-15% that the amount ranges of peptizing agent is preferably; When being peptizing agent with calcium chloride, the 8%-20% that the amount ranges of peptizing agent is preferably.
3. the preparation method of a kind of bentonite inorganic gel according to claim 1 is characterized in that the gel condition of bentonite inorganic gel can be disperseed (4000～20000 rev/mins were disperseed 1～10 minute) for reacting by heating (70～90 ℃ following stirring reaction 1～2 hour) or at a high speed even matter.
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| CN102259881A (en) * | 2011-06-20 | 2011-11-30 | 浙江丰虹新材料股份有限公司 | Method for preparing high-viscosity organic bentonite by virtue of calcium-based bentonite |
| CN104478238A (en) * | 2014-12-17 | 2015-04-01 | 苏州中材非金属矿工业设计研究院有限公司 | Bentonite-based mineral gel and preparation method thereof |
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| CN108190902A (en) * | 2018-01-24 | 2018-06-22 | 安徽国创非金属矿业科技有限公司 | A kind of method that calcium-base bentonite makes inorganic gel sodium |
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| CN102259881A (en) * | 2011-06-20 | 2011-11-30 | 浙江丰虹新材料股份有限公司 | Method for preparing high-viscosity organic bentonite by virtue of calcium-based bentonite |
| CN102259881B (en) * | 2011-06-20 | 2013-03-20 | 浙江丰虹新材料股份有限公司 | Method for preparing high-viscosity organic bentonite by virtue of calcium-based bentonite |
| CN104903415A (en) * | 2013-01-07 | 2015-09-09 | 三菱电机株式会社 | Coating composition, method for producing same, and coated article |
| US9528020B2 (en) | 2013-01-07 | 2016-12-27 | Mitsubishi Electric Corporation | Coating composition, method for producing same, and coated article |
| CN104903415B (en) * | 2013-01-07 | 2017-02-15 | 三菱电机株式会社 | Coating composition, method for producing same, and coated article |
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| CN104477929A (en) * | 2015-01-06 | 2015-04-01 | 山西金宇科林科技有限公司 | Method for preparing high-solid-content and low-viscosity kaolin slurry |
| CN108190902A (en) * | 2018-01-24 | 2018-06-22 | 安徽国创非金属矿业科技有限公司 | A kind of method that calcium-base bentonite makes inorganic gel sodium |
| CN108083291A (en) * | 2018-01-31 | 2018-05-29 | 安徽国创非金属矿业科技有限公司 | A kind of method for improving bentonite inorganic gel yield |
| CN110054194A (en) * | 2018-09-30 | 2019-07-26 | 中国地质大学（北京） | A kind of inorganic gel materials and preparation method thereof |
| CN112007607A (en) * | 2020-05-15 | 2020-12-01 | 苏州国建慧投矿物新材料有限公司 | Bentonite mineral gel for water treatment and its preparation method |
| CN111807381A (en) * | 2020-07-28 | 2020-10-23 | 内蒙古蒙兴粘土科技有限责任公司 | Preparation method of natural montmorillonite mineral inorganic gel |
| CN111825099A (en) * | 2020-09-09 | 2020-10-27 | 苏州国建慧投矿物新材料有限公司 | Aluminum magnesium silicate inorganic gel and preparation method thereof |
| CN113620305A (en) * | 2021-08-25 | 2021-11-09 | 苏州欧亦博工业科技有限公司 | Preparation process of sodium modified bentonite |
| CN115041107A (en) * | 2022-06-01 | 2022-09-13 | 芜湖硕华新材料科技有限公司 | Preparation method of temperature-resistant salt-tolerant high-performance inorganic gel |
| CN115260592A (en) * | 2022-08-02 | 2022-11-01 | 浙江丰虹新材料股份有限公司 | Preparation method of nano organic clay compound for polymer |
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