CN100509163C - Alkaline calcium bentonite and preparation method thereof - Google Patents
Alkaline calcium bentonite and preparation method thereof Download PDFInfo
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- CN100509163C CN100509163C CNB200510101332XA CN200510101332A CN100509163C CN 100509163 C CN100509163 C CN 100509163C CN B200510101332X A CNB200510101332X A CN B200510101332XA CN 200510101332 A CN200510101332 A CN 200510101332A CN 100509163 C CN100509163 C CN 100509163C
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Abstract
The invention discloses an alkaline calcium bentonite and making method, which comprises the following steps: adapting active carclazyte and calcium oxide as raw material; mixing the raw material evenly; reacting the calcium oxide and water to produce calcium hydroxide; diffusing the calcium hydroxide in the active carclazyte layers; reacting one of two oxyhydrogen base with hydrogen of active carclazyte to produce the alkaline calcium bentonite with anion exchanging function. The invention can react with organic acid to prepare composite layered nanometer material, which can be applied in the coating, plastic and new adsorptive material domain.
Description
Technical field
The present invention relates to a kind of active bentonite, particularly have alkaline calcium bentonite of anion exchange capacity and preparation method thereof.
Background technology
Bentonite is a kind of stratified material with cation exchange capacity (CEC), and its main component is an alumino-silicate.Natural montmorillonite mostly is calcium-base bentonite greatly, calcium-base bentonite and modified product thereof have functions such as dilatancy, hydrophily, adsorptivity, cation exchange, catalytic activity, dispersed and suspension, prevent sinking at the mineral oil and the thickening tackify of vegetable and animals oils decolouring, coating, aspects such as the modulation of oil drilling mud, wastewater treatment, Preparation of Catalyst are widely used.But because it does not possess the anion exchange function, purposes is restricted.Hydrotalcite then is the stratified material that another kind has anion exchange capacity, can be used for handling waste water, aspects such as preparation catalyst and complex layered nano material, because that natural water talcum reserves reach impurity less is many, mainly at present adopts artificial synthetic method preparation.Artificial synthetic hydrotalcite-based compound (being called for short HTLds), its advantage is that impurity is few, anion-exchange capacity is high and interlayer exchanges the material that dissimilar anion can obtain different performance, but since its interlamellar spacing little, have acid condition lower skeleton instability and the more high weak point of production cost, influenced its use.In order to make the bentonite exchange capacity better, people have found out many methods, change calcium-base bentonite into sodium bentonite, perhaps its modification are become the organobentonite of high value, have reported some method of modifying as open source literature, and we take passages as follows by retrieval:
1, [autograph] artificial sodium bentonite [author] Han Xiushan [mechanism] Jilin [periodical name] petrochemical technology and application 2005,23 (1) .-47-47[digests] natural bentonite (Bentonite) overwhelming majority (world 70%～80%, China 90%) be calcium-base bentonite, performance is than sodium bentonite difference, and factory is modified as sodium bentonite with artificial natridization's method with calcium-base bentonite usually.For ease of using, often sodium bentonite is divided into artificial sodium bentonite and natural sodium bentonite.Press the kind and the content of exchangeable cations between montmorillonite layer, alkaline coefficient more than or equal to 1 be sodium bentonite, less than 1 be calcium-base bentonite.
2, [autograph] bentonite activation processing and with the resource and environment engineering colleges of [mechanism] Wuhan University of Technology such as research [author] Li Ye Lu Wei of the purple mechanism of action of alkalescence, [periodical name] mining metallurgical engineering .2001,21 (3) .-63-65[digests] calcium-base bentonite is by acid activation, thermal activation, TiCl
4Activation, hydroxy Al and AlCl
3Activation is handled basic purple dye solution, finds to use TiCl
4And AlCl
3The bentonite of activation reaches respectively more than 89% and 98% the basic purple dye rate of taking off, and significantly improves than original soil percent of decolourization; Find by X-ray analysis: TiCl
4And AlCl
3The bentonite of activation has than large interlamellar spacing, and absorption property obviously improves.Modified alta-mud mainly is to have divided and bentonite clay particle generation co-precipitation by cation exchange effect and dyestuff when adsorbing alkaline purple solution.
3, [autograph] modified alta-mud is wished the .1999 of Environmental Pollution and Control of Environmental Science and Engineering system of ten thousand rocs [mechanism] Tsing-Hua University [periodical name] to J acid solution and waste liquor treatment effect [author] Ji Jingping, 21 (6) .-12-14[digests] studied the treatment effect of modified alta-mud to J acid solution and J acid waste liquor, the result shows, modified alta-mud is better than the sour waste liquor of J to the treatment effect of J acid solution, removal effect to J acid waste liquor is relevant with pH and sodium sulphate content, under neutrality or weak basic condition, sodium sulphate content is low more.Clearance to J acid waste liquor is high more, can reach about 50%.
4, [autograph] acid, alkali are to the material physical chemistry research institute of influence [author] Zhou Kaiting [mechanism] Huaqiao University of sodium bentonite suspension system pH value [periodical] Huaqiao University's journal: natural science edition .1998,19 (1) .-40-43[digests] by testing the method for pH value and electrical conductivity, the research sodium montmorillonite forms mass fraction in the acid of pH=1-3, alkali systems when being 0.1% suspension system, the variation behavior of sodium montmorillonite-aqueous systems pH value.The sodium montmorillonite suspension system presents buffering character, keeps the ability of pH value to be decided by that the pH value of the suspension system that it forms is big or small in neutral aqueous solution.The pH value stabilization of suspension system needs the time of 7d approximately, in ageing time, is acid its pH value of suspension system and gos up, and is the suspension system of alkalescence, and its pH value falls after rise.
5, Chinese patent [application (patent) number] CN88100011.6[title] produce the retrofit production method of sodium bentonite of method [application (patent right) people] CFS of Zhou Yunchen [address] Xinyang, Henan Province level bridge town, county parent company of overseas Chinese federation [summary] with the calcium-base bentonite sodium bentonite, belong to the deep process technology of bentonite material.Mainly be applicable to natural calcium-base bentonite is become sodium bentonite with the artificial modification.Core of the present invention is that the calcium bentonite ore deposit with natural saturated humidity adds light ash under the condition of pressure and shearing deformation, carries out exchange reaction fast and generates sodium bentonite.Make the calcium-base bentonite ore deposit of China's abundant adopt this law to generate the sodium bentonite product, remedied deficiency with multipurpose and in great shortage natural sodium bentonite of high-quality.This law is suitable for factory's serialization produces, and cost is low, is better than the production method that adopts at present both at home and abroad.[principal claim] a kind of sodium bentonite production method, add soda ash stirring-extruding-drying-abrasive dust-packing by ore dressing-fragmentation and constitute, it is characterized in that: (1) selects natural bentonite saturated humidity for use, and its water content is 30-50%, contain montmorillonite greater than 65%, with Ca
2+Ion is main, burning into sand stone not, (2) granularity after the fragmentation should be less than 1 centimetre, (3) add light ash 1-3%, soda ash should meet G B210--63 standard, and makes granularity less than 20 mesh sieves through pulverizing, and stir in the double helix mixer (4), (5) in the double helix reactor, pressure is 50～150Kg/Cm
2The detrusion condition under carry out exchange reaction, generate sodium bentonite, the exchange reaction formula is: Ca
2+-bentonite+Na
2CO
3→ 2Na
+-bentonite+CaCO
3
6, Chinese patent [application (patent) number] CN97103231.9[title] a kind ofly exhale Qing Lu Inner Mongol mineral products experimental study institute [summary] to the invention belongs to bentonitic deep process technology with the southern tearoom in process for producing sodium-base bentonite from calcium-base bentonite [application (patent right) people] Sun Zhong [address] Hohhot City ,Inner Mongolia Autonomous Region.Mainly be applicable to the natural calcium base bentonite is modified as sodium bentonite by artificial " dry method ".Its core be only with a disposable realization ion-exchange reactions of Raymond mill with remove two purposes of impure mineral, generate sodium bentonite quickly and easily.Realized factory's serialization production fully, operation is short, cost is low, economic worth is high, is better than the production method that adopts at present both at home and abroad.[principal claim] a kind of process for producing sodium-base bentonite from calcium-base bentonite of using, by select materials-airing-add ground caustic mill-packing constitutes, it is characterized in that: (1) selects for use colloid index greater than 50ml/15g, expansion capacity is greater than the natural calcium base bentonite of 4ml/g; (2) raw material should be between 13%～18% through the moisture content after the airing, and lumpiness should be less than 1 centimetre; (3) add light ash 2～3.5%, soda ash should meet GB210-89 standard, and crosses 20 mesh sieves; (4) light ash fully mixes simultaneously by moisture content dissolving residual in the raw material with raw material in Raymond mill, standing to finish ion-exchange reactions fast under the spreading distortion temperature that also the sensing device operation is produced, generate sodium bentonite, send in the packaging bag through selection by winnowing with the wind-force that can control product granularity.
7, Chinese patent [application (patent) number] CN02103804.X[title] dry-process method for producing bentonite [application (patent right) people] a kind of dry-process method for producing bentonite in Capital Iron ﹠ Steel General Co [address] Shijingshan District, Beijing [summary].The main organobentonite that the natural calcium base bentonite is become high value by the artificial modification that is suitable for.Core of the present invention is that the natural calcium base bentonite is added soda ash in mixing facilities, and exchange reaction generates sodium bentonite; Add activator then, mixing, reaction; Add organic coverture again, fully heating, mixing, reaction are extruded into bar with screw extruder at last, and extrudate drying, abrasive dust become the organobentonite powder.It is simple that it has technology, need not wash and dewater, and the production efficiency height, cost is low, is convenient to advantages such as large-scale production.[principal claim] 1, a kind of dry-process method for producing bentonite, comprise ore dressing-fragmentation-selected-add alkali-mix-add activator-add coverture-heating mixing-extruding-drying-abrasive dust-packaging process, it is characterized in that: the natural calcium base bentonite is added soda ash in mixing facilities, and exchange reaction generates sodium bentonite; Add activator then, mixing, reaction; Add organic coverture again, fully heating, mixing, reaction are extruded into bar with screw extruder at last, and extrudate drying, abrasive dust become the organobentonite powder.
8, the special journal .1996 of the preparation of [autograph] bentonite and application [author] Song Kaiping [periodical name] Mianyang farming, 13 (4) .-22-25, the 46[digest] natural montmorillonite carries out obtaining a kind of thixotropic additive after the modification with the compound of some organic cation compound or organic cation-organic anion, be used for organic liquid and make thickener, dispersant coagulates agent and suspension stabilizer, be mainly used in oil drilling, paint, printing ink, lubricating grease etc.
9, environmental science system of [mechanism] Zhejiang University such as collaborative suction-operated of [autograph] the moon-cation organobentonite and mechanism research [author] Zhu Lizhong Soviet Union rubine thereof, [periodical name] China Environmental Science .2001,21 (5) .-408-411[digests] synthetic and studied suction-operated and the mechanism thereof of a series of the moon-cation organobentonite to phenol, benzene in the water.The result shows that the moon-cation organobentonite has collaborative suction-operated to organic matter in the water, and the property of all kinds of, composition, proportioning and the organic matter itself of its effect size used surfactant during with modification is relevant; Pyrogentisinic Acid's absorption accords with Langmuir and Freundlich adsorption isotherm, be distributional effects (partition) and surface absorption (adsorption) coefficient result, the increase of the contribution rate of distributional effects anion surfactant addition during with modification increases; Based on distributional effects, distribution coefficient is greater than original soil and single cation organobentonite to the absorption of benzene in the water, and is proportionate with organic carbon content.
10, Chinese patent [application (patent) number] CN94110894.5[title] a kind of method of method [application (patent right) people] southern suburbs, Changsha, Hunan lengthization institute of Changsha Chemical Mining Design Inst., Ministry of Chemical Industry [address] [summary] of producing atlapulgite with sodium bentonite with sodium bentonite production atlapulgite, be that the sodium bentonite raw ore is put in the separator that fills magnesium sulfate solution, clean through stirring, then slip is dropped into retort, change stirring pool again over to, add the proper amount of clear water dilution, stir, enter filter press, send into oven drying after changing filter residue over to the slurrying pond, take out siccative through grinding, get final product the high-quality atlapulgite.The atlapulgite quality height that the present invention produces low-grade sodium bentonite, sand content is low, percent of decolourization reaches 100%, activity degree〉220, be applicable to and produce the amiantuhs goods.[principal claim] produces the method for atlapulgite with sodium bentonite, it is characterized in that: the sodium bentonite raw ore is directly put in the separator that fills the auxiliary agent magnesium sulfate solution, clean through stirring, then slip is changed over to and carry out priming reaction in the retort, change stirring pool again over to, add the proper amount of clear water dilution, stir, enter filter press and filter, change filter residue the slurrying washing of over to slurrying pond, the gained slip is sent into oven drying after filtering once more, take out in material through the grinder abrasive dust, promptly get the high-quality atlapulgite, filtrate still can be used as adjuvant water solution and recycles after replenishing a small amount of magnesium sulfate.
Recognize from above-mentioned result for retrieval, the open source literature introduction mainly be to change calcium-base bentonite into sodium bentonite, perhaps its modification is become organobentonite, do not mention the bentonite modified content that becomes with anion exchange capacity, and the Bentonite Modification Technologies production technology that document is introduced is complicated, need to propose acid activation, thermal activation, TiCl as document 2
4Activation, hydroxy Al and AlCl
3Steps such as activation, though the method that has is not difficult, equipment investment is bigger, proposes to need Raymond mill or mixing facilities as document 6 and 7, resulting cost is also higher.The production process that has also may produce pollution.
Summary of the invention
The inventor on the basis of modified alta-mud, adopts the source abundant raw material, equipment is simple and the method for operation simple and feasible, prepares higher, the broad-spectrum alkaline calcium bentonite with anion exchange capacity of a kind of activity after research and testing.
The preparation method of alkaline calcium bentonite of the present invention be with atlapulgite calcium hydroxide with or calcium oxide (because calcium oxide in water, generate calcium hydroxide) be raw material, in the presence of water atlapulgite and calcium hydroxide and or the calcium oxide hybrid reaction obtain, concrete technology is to be that the water of 1～6 times of atlapulgite quality mixes with activity degree 150～350, granularity 60～200 purpose atlapulgites and consumption, makes pulpous state; 20～50% calcium hydroxides that add quantity in the above-mentioned slurry and be the atlapulgite quality with or calcium oxide, mix and obtain reacting raw material; To react raw material and pave, thickness is at 3～30mm, and reaction obtained reacting grog in 10～36 hours under 40～80 ℃; The reaction grog washes with water, removes unreacted calcium hydroxide, and to obtain anion-exchange capacity (with hydrochloric acid neutralisation mensuration) be the alkaline calcium bentonite of 1.0～3.0mmol/g to drying then.
Among the preparation method of alkaline calcium bentonite of the present invention, the raw material atlapulgite is that sulfuric acid process or hydrochloric acid method prepare, its preparation method has had introduction in many open source literatures, the atlapulgite that the present invention uses is mainly emphasized activity degree, its activity degree should be 150～350, the activity degree assay method adopts the hydrogen in the sodium ion exchange activity carclazyte in the sodium acetate solution, determines with the amount of alkali mensuration acetate then.
Calcium oxide popular name of the present invention is a quick lime, and the purity of CaO is greater than 90% (mass content); The calcium hydroxide popular name is a white lime, Ca (OH)
2Purity greater than 90% (mass content).
The reaction mechanism of alkaline calcium bentonite of the present invention is to work as atlapulgite and calcium hydroxide (if adding calcium oxide, calcium oxide generates calcium hydroxide with water earlier) after mixing under the condition that water exists, calcium hydroxide diffuses into the atlapulgite interlayer, the hydroxyl in its two hydroxyls and the hydrogen of atlapulgite react, and obtain alkaline calcium bentonite.Product detects through infrared spectrum and X-ray diffraction, has tradable hydroxyl, and interlayer structure is identical with calcium-base bentonite.
The alkaline calcium bentonite that the present invention prepares is compared with artificial synthetic hydrotalcite compounds, and the alkaline calcium bentonite interlamellar spacing is big, can use under strong acid condition, the more important thing is 20% of the not enough hydrotalcite-based compound of preparation cost; Compare with existing modified alta-mud, alkaline calcium bentonite has well behaved anion exchange function, remedied original bentonitic deficiency, also modified alta-mud character and the purposes with existing open source literature introduction is different, and bentonitic application is widened greatly.
The alkaline calcium bentonite that the present invention prepares, can be directly used in fruit juice, plant wet goods edible liquid depickling, decolour and help filter, the purification of air and water quality, or Preparation of catalysts etc., also can prepare complex layered nano material, be used for fields such as coating, plastics and novel absorption material with organic acid reaction.
The specific embodiment
Embodiment 1
The atlapulgite that makes with activity degree 240, granularity 60 orders, by sulfuric acid process and consumption are that the water of 3 times of atlapulgite quality mixes, and make pulpous state; Adding quantity in the above-mentioned slurry is 30% calcium oxide (CaO purity is greater than 95%) of atlapulgite quality, mixes and obtains reacting raw material; To react raw material and pave, thickness is at 10mm, and reaction obtained reacting grog in 15 hours under 50 ℃; The reaction grog washes with water, removes unreacted calcium hydroxide, and drying obtains the alkaline calcium bentonite that anion-exchange capacity is 1.5mmol/g.
Embodiment 2
The atlapulgite that makes with activity degree 245, granularity 100 orders, by sulfuric acid process and consumption are that the water of 4 times of atlapulgite quality mixes, and make pulpous state; Adding quantity in the above-mentioned slurry is the 42% calcium hydroxide (Ca (OH) of atlapulgite quality
2Purity is greater than 90%), mix and obtain reacting raw material; To react raw material and pave, thickness is at 5mm, and reaction obtained reacting grog in 18 hours under 60 ℃; The reaction grog washes with water, removes unreacted calcium hydroxide, and drying obtains the alkaline calcium bentonite that anion-exchange capacity is 1.8mmol/g.
Embodiment 3
The atlapulgite that makes with activity degree 270, granularity 150 orders, by the hydrochloric acid method and consumption are that the water of 2 times of atlapulgite quality mixes, and make pulpous state; Adding quantity in the above-mentioned slurry is 40% calcium oxide (CaO purity is greater than 90%) of atlapulgite quality, mixes and obtains reacting raw material; To react raw material and pave, thickness is at 5mm, and reaction obtained reacting grog in 18 hours under 50 ℃; The reaction grog washes with water, removes unreacted calcium hydroxide, and drying obtains the alkaline calcium bentonite that anion-exchange capacity is 2.5mmol/g.
Embodiment 4
The atlapulgite that makes with activity degree 260, granularity 100 orders, by the hydrochloric acid method and consumption are that the water of 4 times of atlapulgite quality mixes, and make pulpous state; Adding quantity in the above-mentioned slurry is the 30% calcium hydroxide (Ca (OH) of atlapulgite quality
2Purity is greater than 90%), mix and obtain reacting raw material; To react raw material and pave, thickness is at 8mm, and reaction obtained reacting grog in 12 hours under 70 ℃; The reaction grog washes with water, removes unreacted calcium hydroxide, and drying obtains the alkaline calcium bentonite that anion-exchange capacity is 2.0mmol/g.
Claims (2)
1, a kind of preparation method of alkaline calcium bentonite, it is characterized in that adopting activity degree 150～350 atlapulgite and calcium hydroxide and or calcium oxide be raw material, in the presence of water with atlapulgite and calcium hydroxide and or the calcium oxide hybrid reaction obtain, its preparation technology is as follows:
(1) water of atlapulgite with 1～6 times of quality is mixed, make pulpous state;
(2) add in the above-mentioned slurry quantity be atlapulgite quality 20～50% calcium hydroxide with or calcium oxide, mix and obtain reacting raw material;
(3) will react raw material and pave, thickness is at 3～30mm, and reaction obtained reacting grog in 10～36 hours under 40～80 ℃;
(4) the reaction grog washes with water, removes unreacted calcium hydroxide, and drying obtains alkaline calcium bentonite.
2, the preparation method of alkaline calcium bentonite according to claim 1 is characterized in that the raw material atlapulgite is that sulfuric acid process or hydrochloric acid method prepare granularity at 60～200 purpose atlapulgites; The purity of calcium oxide or calcium hydroxide is greater than 90%.
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