CN100590072C - Method for producing sodium bentonite with calcium bentonite - Google Patents
Method for producing sodium bentonite with calcium bentonite Download PDFInfo
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- CN100590072C CN100590072C CN200710004960A CN200710004960A CN100590072C CN 100590072 C CN100590072 C CN 100590072C CN 200710004960 A CN200710004960 A CN 200710004960A CN 200710004960 A CN200710004960 A CN 200710004960A CN 100590072 C CN100590072 C CN 100590072C
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- bentonite
- sodium bentonite
- dewatering
- calcium
- sodium
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- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 title claims description 39
- 229910000280 sodium bentonite Inorganic materials 0.000 title claims description 39
- 229940080314 sodium bentonite Drugs 0.000 title claims description 39
- 229910000281 calcium bentonite Inorganic materials 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 66
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 31
- 239000000440 bentonite Substances 0.000 claims abstract description 31
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000002689 soil Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 229940092782 bentonite Drugs 0.000 claims description 26
- 238000005189 flocculation Methods 0.000 claims description 22
- 230000016615 flocculation Effects 0.000 claims description 21
- 238000007634 remodeling Methods 0.000 claims description 20
- 229920001661 Chitosan Polymers 0.000 claims description 19
- 239000011734 sodium Substances 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 241001460678 Napo <wasp> Species 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 230000003020 moisturizing effect Effects 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052901 montmorillonite Inorganic materials 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 235000017550 sodium carbonate Nutrition 0.000 abstract description 2
- 230000003311 flocculating effect Effects 0.000 abstract 3
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000003607 modifier Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 208000005156 Dehydration Diseases 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 5
- 125000002091 cationic group Chemical group 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 229910021647 smectite Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 229920002683 Glycosaminoglycan Polymers 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- -1 aluminum (magnesium) oxygen Chemical compound 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a method for preparing na-bentonite using ca-bentonite, which comprises the following steps: pulverized ca-bentonite raw mine soil is added into the water solution which the dispersing agent (NaPO3) 6 is already added, and are immersed, stirred and mixed evenly, then the modifier Na2CO3 is added to the saturated water solution; finally the working procedure of stirring andaging, heating and modifying, high speed dispersion, siphon and impurity removal, centrifugally purifying, flocculating and dewatering are performed in order to obtain the na-bentonite with high quality; the purifying and the modifying working procedure are performed at the same time, and the purifying operation passes through the whole working flow, thus na-bentonite with high quality and high purity comprising very high content of montmorillonite can be obtained. With flocculating and dewatering, the preparing method of the invention has the advantages that the problem of dewatering difficulty for wet modifying is effectively resolved, and the water after flocculating and dewatering is very convenient for recovery, thus the water consumption, the energy consumption and the processing time during drying in the wet modifying process are greatly decreased.
Description
Technical field
The present invention relates to a kind of nonmetal wilkinite raw ore deep process technology, referring in particular to retrofits the natural calcium base bentonite to purify with artificial wet method synchronously prepares the method for sodium 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.Wilkinite is to contain the clay of smectite type mineral, the montmorillonite crystal is formed by two-layer silicon-oxy tetrahedron therebetween layer of aluminum (magnesium) oxygen (hydrogen-oxygen) is octahedra, belong to 2: 1 type lamellar aluminosilicates, there is a spot of silicon to be replaced in the tetrahedron by aluminium, there is a spot of aluminium to be replaced in the octahedron by magnesium, make to produce permanent negative charge between crystal layer, thereby between crystal layer, adsorb a large amount of tradable positively charged ions.According to the difference of the cation type that adsorbs between montmorillonite layer, wilkinite can be divided into 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% be calcium-base bentonite, natural sodium bentonite is seldom.The kind of known exchangeable cation and exchange capacity (CEC) have much relations: high-valence cationic (Ca
2+, Mg
2+Deng) hydration shell is thin, expansion multiple is low, CEC is little; And low price positively charged ion (Na
+, K
+Deng) aquation thickness, expansion multiple height, CEC be big, visible sodium ion has stronger hydration than calcium ion.Therefore, sodium bentonite has more superior physical and chemical performance than calcium-base bentonite, and is big as water-intake rate, expansion multiple is high, cation exchange capacity is big, oilness is good, Heat stability is good and have stronger plasticity-and cementability etc.Therefore, the sodium modification of calcium-base bentonite is one of effective way that improves its using value and economic worth.
The sodium modification principle of calcium-base bentonite is to utilize the cationic exchange of calcium-base bentonite, the Ca between cheating engaging layer
2+Run into certain density Na
+The time just following reaction can take place, thereby be translated into sodium bentonite.
Ca-bentonite+2Na
+→Na-bentonite+Ca
2+
Sodium modification technology has two kinds of dry method and wet methods, and dry method remodeling technology has duplex extrusion method, stockyard method, spiral choked flow extrusion process etc.Its cardinal principle is to add dissolved sodium salt (often be yellow soda ash, sodium-chlor or Sodium hexametaphosphate 99 etc. are also arranged) in the wilkinite siccative, by the extruding that adds the high-energy mechanical force with Na
+Force to introduce between montmorillonite layer.This method difficulty makes the abundant sodium of wilkinite, and gained sodium bentonite purity is not high.Wet method remodeling technology claims suspension method again, promptly adds the continuous heated and stirred of excessive sodium salt in water medium, makes montmorillonite fully disperse, expand and realizes sodium.This method quality product is more stable, obtains high quality, high purity sodium bentonite easily, but product dehydration, dry difficult.
Number of patent application CN85105253 has invented a kind of method that is obtained sodium bentonite by calcium-base bentonite in certain pressure down cut distortion generation ion-exchange.Though this method can realize working continuously well, also exists following defective: 1, required equipment is more, technology is loaded down with trivial details.Equipment such as this arts demand mixing machine, screw extrusion press, roasting kiln, whizzer, lift, winnowing type pulverizer obtain product through more than 30 steps.2, higher to ingredient requirement.It is water content about 10% and the particle diameter calcium-base bentonite dry powder grain less than 4mm that this technical process requires raw material.3, quality product is difficult to control.The method of this process using shearing strain realizes ion-exchange, is difficult to guarantee good remodeling effect, and does not remove SiO in the flow process
2Steps necessary Deng impurity.
Number of patent application CN88100011 improves the method for number of patent application CN85105253.This method is saved large number quipments such as secondary breaker, whizzer, has simplified technical process, takes comparatively easy method to realize remodeling.But this method adopts the method for shearing strain to realize ion-exchange equally, still can not guarantee quality product.And this method is also very harsh to ingredient requirement: require the raw ore of calcium base bentonite smectite content greater than 65%, the interchangeability positively charged ion is with Ca
2+Be main and do not contain sandstone, and the known sandstone (SiO that removes in the wilkinite
2) impurity also very the difficulty.
Number of patent application CN97103231.9 utilizes Raymond mill shearing strain that calcium-base bentonite is realized the disposable generation sodium bentonite of ion-exchange.Though this method technology is simple, with low cost, its quality product also is difficult to control, the sodium bentonite smectite content after retrofiting with this method only about 70%.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method for producing sodium bentonite with calcium bentonite of using, and this method for preparing sodium bentonite can overcome " dry method "---and shearing method prepares the defective that the sodium bentonite quality product is difficult to control, impurity is difficult to remove.The present invention has adopted the method that wet method is retrofited and purification is carried out simultaneously, the slurries flocculation dewatering prepares sodium bentonite, has increased the steps necessary of removing impurity.And adopt the flocculation dewatering method to solve the difficult problem of wet method remodeling dehydration effectively, thereby realized that less energy-consumption, low cost, high-level efficiency prepare high-quality high pure sodium base bentonite.
The technical problem to be solved in the present invention is realized by following scheme: the present invention is made up of operations such as slurrying, remodeling, purification, dehydrations, and wherein the step of removal of impurities purification runs through whole process flow, to guarantee quality product.Dispersion agent (the NaPO that in the pure water of 1000 parts of weight, adds 1～1.5 part of weight
3)
6After the stirring and dissolving, the raw ore of calcium base bentonite soil weight that is crushed to particle diameter 1～2cm is 200～300 parts joins in the above-mentioned solution, mix after the immersion disintegration, in the above-mentioned system that has mixed, add the remodeling agent Na of 10～12 parts of weight then
2CO
3Saturated aqueous solution, stir ageing make it thorough mixing after 18～24 hours decant remove lower floor's large granular impurity, then the upper strata mixed solution being heated to the also in good time moisturizing of 70～90 ℃ of violent stirring fully reacted it 1～2 hour, leave standstill decant except that behind the sub-cloud residue, in high speed dispersor, disperseed 0.5～1 hour, system after the high speed dispersion is diluted 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, upper strata ore pulp centrifugation is obtained the sodium bentonite concentrate slurry, the low-grade thin slag of the lower floor that obtains simultaneously reclaims again purifies, it is that to be made into mass concentration in 5% the aqueous acetic acid be 0.5% chitosan aqueous acetic acid that chitosan is joined mass concentration, with this solution above-mentioned sodium bentonite concentrate slurry is carried out flocculation dewatering, the i.e. flocculation agent chitosan aqueous acetic acid that has prepared to its continuous adding, in the process that adds flocculation agent, be that the adjusting of 5～10mol/L NaOH solution makes the pH value stabilization of system more than 7 with concentration simultaneously in good time, the chitosan aqueous acetic acid volume that adds is 7%～9% o'clock of sodium bentonite concentrate slurry volume, sodium bentonite flocculates fully, and suction filtration dehydration after drying is pulverized and obtained high-grade sodium bentonite powder then.
Below be schematic illustration of the present invention:
The technology that the present invention adopts is that wet method remodeling carries out simultaneously with wet purification, compare with dry method, 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, thereby can obtain than the better remodeling effect of dry method.In addition, because the carrying out of natridization reaction further improved montmorillonite expansion dispersive ability again, 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, therefore can obtain comparatively ideal refining effect with the impure mineral that does not reach the micelle level.
For the difficult problem of the dehydration of serious restriction wet method retrofit application, the present invention adopts the flocculation dewatering method to be solved.Calcium-base bentonite is after remodeling is purified, and the sodium bentonite concentrate slurry that obtains has formed stable colloidal solution, and the dewatering of these slurries mainly contains filter press technique, vacuum blade suction filtration, direct heating oven drying method, supercentrifugal process etc.But because the energy consumption that has in these methods is bigger, the technology that has is loaded down with trivial details, and what have has relatively high expectations to equipment performance, and its effect and efficient are all undesirable.The method characteristics low because of its energy consumption, that equipment is little, efficient is high of adding flocculation agent become one of prefered method of slurries dehydration.
The mechanism of flocculation dewatering is to add a certain amount of chemical substance---flocculation agent in the bentonite slurry that forms stable colloidal solutions, destroys colloidal stability, the flocs unit that colloidal solid is gathered into have separable character, and suction filtration gets the wilkinite solid again.The present invention selects for use chitosan as flocculation agent, chitosan, and promptly (1,4)-2-amino-2-deoxidation-β-D dextran is a kind of cationic straight chain glycosaminoglycan, is chitin is sloughed the N-ethanoyl through the concentrated base heat treated product.Chitosan is as a kind of novel organic polymer coargulator,, readily biodegradable natural, nontoxic with it, the harmless good characteristic of human body gained great popularity.Its flocculation mechanism mainly is: (1) bridging effect: simultaneously in conjunction with a plurality of colloidal solids, chitosan molecule is bound up as " middle bridge " thereby many colloidal solids and makes it to form reticulated structure and precipitate chitosan molecule by ionic linkage and hydrogen bond.(2) charge neutrality effect: chitosan is dissolved in the character that has weak cation in the weak acid, it and electronegative micelle mutually near the time, its lip-deep part negative charge that neutralizes takes off surely micelle, bumps each other and precipitates.Chitosan required for the present invention only needs the special-purpose chitosan of very general flocculation to get final product.
Advantage of the present invention:
1, adopts wet method that calcium-base bentonite is carried out sodium modification, guaranteed stable, good remodeling effect.
2, taked the technology of purifying and retrofiting and carrying out simultaneously, made purification operations run through whole flow process, thereby obtained the very high high-quality sodium bentonite of smectite content.
3, utilize the method for flocculation dewatering to solve the difficult problem of wet method remodeling dehydration well, make that energy consumption and the treatment time in the wet method remodeling drying process descends significantly.
4, simple for process, desired raw material (Na
2CO
3, (NaPO
3)
6, chitosan etc.) cheaply be easy to get.Under the not high situation of cost, can make the fine sodium bentonite.
5, the water behind the flocculation dewatering of the present invention easily reclaims use.Improved the very big shortcoming of wet method remodeling water consumption.
Following Fig. 2, Fig. 3, Fig. 4 are respectively raw ore, X-ray powder diffraction (XRD) collection of illustrative plates of sodium bentonite behind purify remodeling back sodium bentonite, the flocculation dewatering.
Can find that by XRD spectra remodeling back original ore soil exists
001 diffraction peak of the calcium-base bentonite that (Fig. 2 calcium-base bentonite original soil XRD spectrum) located disappears,
(Fig. 3 retrofit back wilkinite XRD spectrum) and
(XRD of soil spectrum behind Fig. 4 flocculation dewatering) locates to occur a sharp-pointed strong peak, and this is the diffraction peak of 001 of typical high-quality sodium bentonite, has as seen realized the sodium modification of calcium-base bentonite fully with preparation method of the present invention.
The strong peak of (Fig. 2) locating and
The spike of (Fig. 2) locating is typical quartzy impurity peaks, behind remodeling
(Fig. 3, Fig. 4) locates more sharp-pointed peak and disappears, and illustrates that most impurity is removed in the process of purifying.Although residual cristobalite content is seldom, because the diffracting power of cristobalite is than strong many of polynite, so
The strong peak at place is still very strong on collection of illustrative plates.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Fig. 2 is raw ore X-ray powder diffraction (XRD) collection of illustrative plates
Fig. 3 is remodeling back sodium bentonite X-ray powder diffraction (XRD) collection of illustrative plates of purifying
Fig. 4 is sodium bentonite X-ray powder diffraction (XRD) collection of illustrative plates behind the flocculation dewatering
Embodiment
Come the present invention is elaborated with a specific embodiment below:
According to technical process of the present invention Xinghe County, Inner Mongol natural calcium base bentonite is purified and sodium modification concrete steps:
1, with 1g dispersion agent (NaPO
3)
6Add in the 800g pure water, after the stirring and dissolving, the raw ore of calcium base bentonite 200g to the about 1cm of particle diameter joins in the above-mentioned solution with coarse crushing, stirring and evenly mixing after the immersion disintegration.
2,8g is retrofited agent Na
2CO
3Add in the above-mentioned mixed system after being made into saturated aqueous solution, stir then and make its thorough mixing ageing 18h.
3, discard lower floor too behind the granule foreign, will go up coating systems and be heated to 90 ℃, violent stirring and moisturizing in good time make system fully react 1h under this temperature.
4, leave standstill discard lower floor's residue after, in high speed dispersor, disperseed 30 minutes.
5, system is diluted to 4 times of original volume, leave standstill 1.5h after stirring a little after, siphon obtains the upper strata ore pulp, discards lower floor's residue.
6, centrifugation (centrifugal speed is 1500rpm) obtains upper strata sodium bentonite concentrate slurry 3800ml, and the low-grade thin slag of the lower floor that obtains simultaneously reclaims again purifies.
7, flocculation agent-chitosan (0.5%) acetic acid (5%) aqueous solution that continuous adding has prepared in the sodium bentonite concentrate slurry that above-mentioned centrifugation obtains, regulate simultaneously making the pH value stabilization of system about 8 in the process that adds flocculation agent with NaOH solution (concentration is 5mol/L), sodium bentonite flocculates fully behind the adding chitosan solution 280ml in good time.The suction filtration back 80 ℃ of drying and crushing of dewatering obtain high-grade sodium bentonite powder 100g then.
Claims (1)
1, uses method for producing sodium bentonite with calcium bentonite, comprise slurrying, remodeling, purification, dehydration procedure, it is characterized in that: the dispersion agent (NaPO that in the pure water of 1000 parts of weight, adds 1～1.5 part of weight
3)
6After the stirring and dissolving, the raw ore of calcium base bentonite soil weight that is crushed to particle diameter 1～2cm is 200～300 parts joins in the above-mentioned solution, mix after the immersion disintegration, in the above-mentioned system that has mixed, add the remodeling agent Na of 10～12 parts of weight then
2CO
3Saturated aqueous solution, stir ageing make it thorough mixing after 18～24 hours decant remove lower floor's large granular impurity, then the upper strata mixed solution being heated to the also in good time moisturizing of 70～90 ℃ of violent stirring fully reacted it 1～2 hour, leave standstill decant except that behind the sub-cloud residue, in high speed dispersor, disperseed 0.5～1 hour, system after the high speed dispersion is diluted 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, upper strata ore pulp centrifugation is obtained the sodium bentonite concentrate slurry, the low-grade thin slag of the lower floor that obtains simultaneously reclaims again purifies, it is that to be made into mass concentration in 5% the aqueous acetic acid be 0.5% chitosan aqueous acetic acid that chitosan is joined mass concentration, with this solution above-mentioned sodium bentonite concentrate slurry is carried out flocculation dewatering, the i.e. flocculation agent chitosan aqueous acetic acid that has prepared to its continuous adding, in the process that adds flocculation agent, be that the adjusting of 5～10mol/LNaOH solution makes the pH value stabilization of system more than 7 with concentration simultaneously in good time, the chitosan aqueous acetic acid volume that adds is 7%～9% o'clock of sodium bentonite concentrate slurry volume, sodium bentonite flocculates fully, and suction filtration dehydration after drying is pulverized and obtained high-grade sodium bentonite powder then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN101823722A (en) * | 2010-05-10 | 2010-09-08 | 内蒙古大学 | Method for preparing bentonite inorganic gel from calcium bentonite |
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| CN116121739B (en) * | 2023-02-22 | 2023-10-13 | 江苏科利恩净水科技有限公司 | Zinc-containing and phosphorus-free iron prefilming agent for weak acid water quality and preparation method thereof |
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