CN1803294A - Alkaline calcium bentonite and its preparation method - Google Patents
Alkaline calcium bentonite and its preparation method Download PDFInfo
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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 invention relates to active bentonite, in particular to alkaline calcium bentonite with anion exchange capacity and a preparation method thereof.
Background
Bentonite is a layered material with cation exchange capacity, and the main component of the bentonite is aluminosilicate. The natural bentonite is mostly calcium bentonite, and the calcium bentonite and modified products thereof have the functions of expansibility, hydrophilicity, adsorptivity, cation exchange property, catalytic activity, dispersibility, suspensibility and the like, and are widely applied to the aspects of mineral oil and animal and vegetable oil decoloration, thickening, tackifying and anti-settling of paint, modulation of oil field drilling mud, wastewater treatment, catalyst preparation and the like. However, since it does not have an anion exchange function, its use is limited. Hydrotalcite is another layered material with anion exchange capacity, can be used for treating wastewater, preparing catalysts, composite layered nano materials and the like, and is mainly prepared by an artificial synthesis method at present due to small reserves and more impurities of natural hydrotalcite. The artificially synthesized hydrotalcite compound (abbreviated as HTLds) has the advantages of less impurities, high anion exchange capacity and capability of exchanging different types of anions between layers to obtain materials with different properties, but the use of the artificially synthesized hydrotalcite compound is influenced due to the defects of small interlayer spacing, unstable skeleton under acidic conditions, high production cost and the like. In order to make the bentonite exchange capacity better, people think of a plurality of methods, namely, calcium bentonite is changed into sodium bentonite, or the calcium bentonite is changed into high-value organic bentonite, for example, the published documents report some modification methods, and the following are extracted by searching:
1. [ PROBLEMS]artificial sodium Bentonite [ authors]Korea-Xiushan [ mechanism]Jilin [ journal]petrochemical technology and application 2005, 23(1). -47-47 [ abstracts]most of Bentonite (Bentonite) in nature (70% -80% in the world, 90% in China) is calcium Bentonite, the performance of which is poorer than that of sodium Bentonite, and a production plant usually modifies the calcium Bentonite into the sodium Bentonite by an artificial sodium modification method. For convenience of application, sodium bentonite is often classified into artificial sodium bentonite and natural sodium bentonite. According to the species and content of exchangeable cations between montmorillonite layers, sodium bentonite with the alkalinity coefficient more than or equal to 1 is used, and calcium bentonite with the alkalinity coefficient less than 1 is used.
2. [ PROBLEMS]Bentonite activation treatment and its mechanism of action with basic violet [ authors]Li, Yanglu, Wei, etc. [ institution]Wuhan university resource and environmental engineering college, [ journal]mining and metallurgy engineering, 2001, 21(3)]-63-65 [ abstracts]calcium bentonite is activated by acid, heat, TiCl4Activated, aluminum hydroxy and AlCl3Activating, treating the basic violet dye solution and discovering with TiCl4And AlCl3The removal rate of the activated bentonite to the basic violet dye reaches more than 89 percent and 98 percent respectively, and the removal rate is higher than the original soil decolorization rateThe improvement is remarkable; by X-ray analysis it was found that: TiCl (titanium dioxide)4And AlCl3Activated bentonite has a large interlamellar spacing,and the adsorption performance is obviously improved. The modified bentonite is mainly subjected to the coprecipitation action with bentonite particles through the cation exchange action and the dye when absorbing the basic violet solution.
3. The results of research on the treatment effect of the modified bentonite on the J acid solution and the J acid waste mother liquor in 21(6) -12-14 [ abstracts]show that the treatment effect of the modified bentonite on the J acid solution is better than that of the J acid waste mother liquor, the removal effect of the modified bentonite on the J acid waste mother liquor is related to pH and sodium sulfate content, and the sodium sulfate content is lower under neutral or alkalescent conditions. The higher the removal rate of the J acid waste mother liquor is, the highest removal rate can reach about 50 percent.
4. Influence of acid and alkali on pH of sodium bentonite suspension system [ authors]zhoukai tin [ mechanism]material physicochemical research institute of university of china [ publication name]proceedings of university of china: 1998, 19(1) -40-43 [ abstracts]the change behavior of the pH value of the sodium montmorillonite-water system is researched by a method for testing the pH value and the conductivity when the sodium montmorillonite forms a suspension system with the mass fraction of 0.1% in an acid and alkali system with the pH value of 1-3. Sodium montmorillonite suspensions exhibit buffering properties and the ability to maintain the pH is determined by the pH of the suspension formed in a neutral aqueous solution. The pH value of the suspension system is stable for about 7 days, and in the aging time, the pH value of the suspension system which is acidic rises, and the pH value of the suspension system which is alkaline falls.
5. Chinese patent application (patent) No. CN88100011.6 name method for producing calcium bentonite sodium bentonite application (patentee) Zhou Yun Chen (Address) Henan province, Xinyang county, bridge and town Union headquarters (Abstract) CFS modified sodium bentonite production method belongs to the deep processing technology of bentonite materials. The method is mainly suitable for artificially modifying natural calcium bentonite into sodium bentonite. The core of the invention is that natural saturated moisture calcium bentonite ore is added with soda powder to carry out exchange reaction rapidly under the condition of pressure shearing deformation to generate sodium bentonite. Makes the rich calcium base of China expandThe method for producing sodium bentonite from the bentonite ore makes up the defects of multipurpose and rare high-quality natural sodium bentonite. The method is suitable for factory continuous production, has low cost, and is superior to the production methods adopted at home and abroad at present. [ PRIMARY]A method for producing sodium bentonite, comprising the steps of mineral separation, crushing, soda addition, stirring, extrusion, drying, grinding and packaging, and is characterized in that: (1) natural bentonite with saturated humidity, water content of 30-50%, montmorillonite content of more than 65%, and Ca content2+Mainly taking ions without sand, 2, reducing the particle size after crushing to less than 1 Cm, 3, adding 1-3% of soda powder, wherein the soda powder meets the GB210-63 standard and is crushed to the particle size of less than 20 meshes, 4, stirring in a double-helix stirring mixer, and 5, in the double-helix reactor, the pressure is 50-150 Kg/Cm2The exchange reaction is carried out under the shearing deformation condition to generate sodium bentonite, and the exchange reaction formula is as follows: 。
6. chinese patent application (patent) No. CN97103231.9 (name) a method for producing sodium bentonite by using calcium bentonite (patent application (patentee) man, Sun Zhong (Address) and inner Mongolia mineral experimental research institute, Calif. Nancha autonomous region and Xinte City Ling Qinglu inner Mongolia mineral research institute, abstract, the invention belongs to the deep processing technology of bentonite. The method is mainly suitable for modifying natural calcium bentonite into sodium bentonite by an artificial 'dry method'. The core is that only one Raymond mill is used for realizing two purposes of ion exchange reaction and removing impurityminerals at one time, and the sodium bentonite is quickly and conveniently generated. Completely realizes the continuous production of factories, has short working procedure, low cost and high economic value, and is superior to the production methods adopted at home and abroad at present. [ PRIOR ART]A method for producing sodium bentonite from calcium bentonite, comprising the steps of selecting materials, airing, adding alkali for grinding and packaging, characterized in that: (1) selecting natural calcium bentonite with colloid value of more than 50ml/15g and expansion capacity of more than 4 ml/g; (2) the water content of the dried raw materials is between 13 and 18 percent, and the block size is less than 1 cm; (3) adding 2-3.5% of soda ash powder, wherein the soda ash is in accordance with the GB210-89 standard, and sieving the soda ash by a 20-mesh sieve; (4) the soda powder is fully mixed with the raw material in the Raymond mill and simultaneously dissolved by residual moisture in the raw material, and the ion exchange reaction is rapidly completed under the conditions of being subjected to rolling deformation and sensing the temperature generated by the operation of equipment to generate sodium bentonite, so that the wind power capable of controlling the product granularity is conveyed into a packaging bag through air separation.
7. Chinese patent application (patent) No. cn02103804.x name method for producing organic bentonite by dry process [ application (patentee)]headquartering company [ address]rocky scenic mountain area of beijing city [ abstract]method for producing organic bentonite by dry process. The method is mainly suitable for preparing high-value organic bentonite from natural calcium bentonite through artificial modification. The core of the invention is that natural calcium bentonite is added with soda ash in mixing equipment for exchange reaction to generate sodium bentonite; then adding an activating agent, uniformly mixing and reacting; addingorganic covering agent, heating, mixing, reacting, extruding with screw extruder to obtain strip, oven drying, and grinding to obtain organobentonite powder. It has the advantages of simple process, no need of washing and dewatering, high production efficiency, low cost, convenient large-scale production, etc. [ claim 1]A method for producing organobentonite by a dry process, comprising the steps of ore dressing, crushing, fine selection, alkali addition, mixing, activating agent addition, covering agent addition, heating and mixing, extrusion, drying, grinding and packaging, and is characterized in that: adding soda into natural calcium bentonite in mixing equipment, and performing exchange reaction to generate sodium bentonite; then adding an activating agent, uniformly mixing and reacting; adding organic covering agent, heating, mixing, reacting, extruding with screw extruder to obtain strip, oven drying, and grinding to obtain organobentonite powder.
8. The title of organic bentonite is "Songyanhe" journal of agricultural Proc. 1996, 13(4) -22-25, 46 "Abstract" natural bentonite is modified with organic cationic compound or organic cationic-organic anionic compound to obtain a thixotropic additive for organic liquid as thickener, dispersant, coagulant and suspension stabilizer, mainly for petroleum drilling, paint, ink, grease, etc.
9. [ PROBLEMS]synergistic adsorption effect and mechanism of anion-cation organobentonite [ Author]Suyuhong, etc. [ institution]department of environmental science at Zhejiang university, [ publication]Chinese environmental science [ 2001, 21(5)]-408-411 [ abstracts]synthesis and research on adsorption effect and mechanism of phenol and benzene in water by a series of anion-cation organobentonites. The result shows that the anion-cation organobentonite has synergistic adsorption effect on the organic matters in water, and the action size of the anion-cation organobentonite is related to various types, compositions and proportions of the used surfactants during modification and the self character of the organic matters; the adsorption to phenol conforms to Langmuir and Freundlich adsorption isotherms and is the result of the joint action of partition action (partition) and surface adsorption (adsorption), and the contribution rate of partition action is increased along with the increase of the addition amount of the anionic surfactant during modification; the adsorption of benzene in water is mainly based on distribution effect, the distribution coefficient is greater than that of the original soil and the single-cation organic bentonite, and the adsorption is positively correlated with the content of organic carbon.
10. Chinese patent application No. CN94110894.5 entitled method for producing activated clay with sodium bentonite, the institute of Changsha chemical mine design of the department of chemical industry, the Address, the Long Sha Ming Hua Ming Ji, the south suburb Long Shih, Hunan province, the abstract is a method for producing activated clay with sodium bentonite, which is characterized in that sodium bentonite raw ore is put into a separator filled with magnesium sulfate aqueous solution, stirred and scrubbed, then the slurry is put into a reaction tank, then transferred into a stirring tank, added with proper amount of clear water for dilution, stirred, transferred into a filter press, transferred into a filter residue pulping tank, dried in a baking oven, taken out and ground to obtain the high-quality activated clay. The invention makes the activated clay produced by low grade sodium bentonite have high quality, low sand content, 100% decolorization rate and more than 220 activity, and is suitable for producing high grade petroleum products. [ PRIOR ART]A process for producing activated clay from sodium bentonite, which comprises the steps of: directly putting the sodium bentonite raw ore into a separator containing an auxiliary agent magnesium sulfate aqueous solution, stirring and scrubbing, then transferring the slurry into a reaction tank for activation reaction, then transferring into a stirring tank, adding a proper amount of clear water for dilution, stirring, filtering in a filter press, transferring the filter residue into a pulping tank for pulping and washing, filtering the obtained slurry again, then sending into a drying furnace for drying, taking out the slurry, grinding the slurry by a grinder to obtain high-quality activated clay, and supplementing a small amount of magnesium sulfate into the filtrate, wherein the filtrate can still be used as the auxiliary agent aqueous solution for recycling.
From the above search results, it is understood that the publications mainly describe the modification of calcium bentonite into sodium bentonite or the modification of sodium bentonite into organic bentonite, there is no mention of modifying bentonite into bentonite having anion exchange capacity, and the bentonite modification method described in the publications is complicated in production process, such as document 2, which requires acid activation, heat activation, TiCl activation4Activated, aluminum hydroxy and AlCl3Some methods, such as activation, have a large equipment investment, although they are not difficult, and documents 6 and 7 propose that a Raymond mill or a mixing device is required, and the total cost is also high. Some production processes may also produce pollution.
Disclosure of Invention
Through research and experiments, on the basis of modified bentonite, the invention adopts a method with rich raw materials, simple equipment and simple and feasible operation to prepare the alkaline calcium bentonite with high activity and wide application and anion exchange capacity.
The preparation method of the alkaline calcium-based bentonite comprises the steps of mixing activated clay calcium hydroxide and/or calcium oxide (calcium hydroxide is generated in water due to calcium oxide) serving as raw materials and reacting the activated clay with the calcium hydroxide and/or the calcium oxide in the presence of water, wherein the specific process comprises the steps of mixing the activated clay with the activity degree of 150-350 and the granularity of 60-200 meshes with water with the amount of 1-6 times of the mass of the activated clay to prepare slurry; adding calcium hydroxide and/or calcium oxide which account for 20-50% of the mass of the activated clay into the slurry, and uniformly mixing to obtain a reaction raw material; paving the reaction raw material to a thickness of 3-30 mm, and reacting at 40-80 ℃ for 10-36 hours to obtain reaction clinker; and washing the reaction clinker with water to remove unreacted calcium hydroxide, and then drying to obtain the alkaline calcium bentonite with the anion exchange capacity (measured by a hydrochloric acid neutralization method) of 1.0-3.0 mmol/g.
In the preparation method of the alkaline calcium bentonite, the raw material of the activated clay is prepared by a sulfuric acid method or a hydrochloric acid method, the preparation method is already introduced in a plurality of published documents, the activated clay used in the method mainly emphasizes the activity degree, the activity degree is 150-350, the activity degree determination method adopts sodium ions in sodium acetate solution to exchange hydrogen in the activated clay, and then alkali is used for determining the amount of acetic acid.
The calcium oxide is commonly named as quicklime, and the purity of CaO is more than 90% (mass content); calcium hydroxide is known by the common name hydrated lime, Ca (OH)2The purity of (A) is more than 90% (mass content).
The reaction mechanism of the alkaline calcium bentonite is that after the activated clay and calcium hydroxide (if calcium oxide is added, the calcium oxide and water generate calcium hydroxide) are mixed under the condition of water existence, the calcium hydroxide diffuses into the activated clay layer, one of two hydroxide radicals reacts with the hydrogen of the activated clay, and the alkaline calcium bentonite is obtained. The product is detected by infrared spectrum and X-ray diffraction, has exchangeable hydroxyl, and has the same interlayer structure as calcium bentonite.
Compared with the artificially synthesized hydrotalcite compound, the alkaline calcium bentonite prepared by the invention has large interlayer spacing, can be used under the condition of strong acid, and more importantly, has the preparation cost less than 20 percent of that of the hydrotalcite compound; compared with the existing modified bentonite, the alkaline calcium bentonite has good anion exchange function, makes up for the defects of the original bentonite, is different from the modified bentonite introduced by the existing open literature in properties and application, and greatly widens the application field of the bentonite.
The alkaline calcium bentonite prepared by the invention can be directly used for deacidification, decoloration and filter aid of edible liquid such as fruit juice, vegetable oil and the like, purification of air and water quality, preparation of a catalyst and the like, can also be reacted with organic acid to prepare a composite layered nano material, and can be used in the fields of coatings, plastics, novel adsorption materials and the like.
Detailed Description
Example 1
Mixing activated clay with activity of 240 meshes and granularity of 60 meshes, which isprepared by a sulfuric acid method, with water the amount of which is 3 times of the mass of the activated clay to prepare slurry; adding 30 percent of calcium oxide (CaO purity is more than 95 percent) of the mass of the activated clay into the slurry, and uniformly mixing to obtain a reaction raw material; paving the reaction raw material to a thickness of 10mm, and reacting at 50 ℃ for 15 hours to obtain reaction clinker; and washing the reaction clinker with water, removing unreacted calcium hydroxide, and drying to obtain the alkaline calcium bentonite with the anion exchange capacity of 1.5 mmol/g.
Example 2
Mixing activated clay with activity of 245 and granularity of 100 meshes, which is prepared by a sulfuric acid method, with water the amount of which is 4 times of the mass of the activated clay to prepare slurry; to the above slurry was added calcium hydroxide (Ca (OH)) in an amount of 42% by mass of activated clay2The purity is more than 90 percent), and the raw materials are uniformly mixed to obtain a reaction raw material; paving the reaction raw material to a thickness of 5mm, and reacting at 60 ℃ for 18 hours to obtain reaction clinker; washing the reaction clinker with water to remove unreacted calcium hydroxide, and drying to obtain anion exchange capacityAn amount of 1.8mmol/g of alkaline calcium bentonite.
Example 3
Mixing activated clay with activity of 270, granularity of 150 meshes and prepared by a hydrochloric acid method with water the amount of which is 2 times of the mass of the activated clay to prepare slurry; adding calcium oxide (CaO purity is more than 95%) with the amount of 40% of the mass of the activated clay into the slurry, and uniformly mixing to obtain a reaction raw material; paving the reaction raw material to a thickness of 5mm, and reacting at 50 ℃ for 18 hours to obtain reaction clinker; and washing the reaction clinker with water, removing unreacted calcium hydroxide, and drying to obtain the alkaline calcium bentonite with the anion exchange capacity of 2.5 mmol/g.
Example 4
Mixing activated clay with the activity of 260 meshes and the granularity of 100 meshes, which is prepared by a hydrochloric acid method, with water the dosage of which is 4 times of the mass of the activated clay to prepare slurry; to the above slurry was added calcium hydroxide (Ca (OH)) in an amount of 30% by mass of activated clay2Purity more than 90 percent) and uniformly mixing to obtain reaction raw material(ii) a Paving the reaction raw material to be 8mm thick, and reacting at 70 ℃ for 12 hours to obtain reaction clinker; and washing the reaction clinker with water, removing unreacted calcium hydroxide, and drying to obtain the alkaline calcium bentonite with the anion exchange capacity of 2.0 mmol/g.
Claims (2)
1. The preparation method of alkaline calcium-based bentonite is characterized in that activated clay and calcium hydroxide and/or calcium oxide are used as raw materials, and the alkaline calcium-based bentonite is obtained by mixing and reacting the activated clay and the calcium hydroxide and/or the calcium oxide in the presence of water, and the preparation process comprises the following steps:
(1) mixing activated clay with water of which the mass is 1-6 times that of the activated clay to prepare slurry;
(2) adding calcium hydroxide and/or calcium oxide in an amount of 20-50% by mass of the activated clay into the slurry, and uniformly mixing to obtain a reaction raw material;
(3) and paving the reaction raw material to a thickness of 3-30 mm, and reacting at 40-80 ℃ for 10-36 hours to obtain reaction clinker.
(4) And washing the reaction clinker with water, removing unreacted calcium hydroxide, and drying to obtain the alkaline calcium-based bentonite.
2. The method for producing an alkaline calcium-based bentonite according to claim 1, wherein the raw material activated clay is an activated clay having an activity of 150 to 350 and a particle size of 60 to 200 mesh, which is produced by a sulfuric acid method or a hydrochloric acid method; the purity of the calcium oxide or calcium hydroxide is more than 90%.
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