CN102716723A - Method for preparing environment-friendly starch/bentonite composite material - Google Patents
Method for preparing environment-friendly starch/bentonite composite material Download PDFInfo
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Abstract
The invention relates to a method for preparing an environment-friendly starch/bentonite composite material. The method is characterized by comprising the following steps: modifying calcium-base bentonite by cation starch, namely fully dispersing the calcium-base bentonite into water, performing washing purification, adding a sodium chloride solution for sodium treatment, then uniformly dispersing the bentonite subjected to sodium treatment into the water, adding the cation starch aqueous solution with a concentration of 1 to 8g/L, controlling the mass ratio of the bentonite subjected to sodium treatment to the solution at 1: (4-8), stirring for 0.5 to 2.5 hours in the water bath at the temperature of 25 to 75 DEG C, performing solid and liquid separation on the product, washing, drying, activating, grinding, screening, and thus obtaining the starch/bentonite composite material. The environment-friendly starch/bentonite composite material is low in cost, high in performance and environment-friendly; compared with the bentonite, the starch/bentonite composite material is changed in the aspect of surface appearance, electric characteristic and interlayer space; the environment-friendly starch/bentonite composite material can remove pollutants such as dye methylene blue, Congo red, p-nitrophenol and hexavalent chromium and is applicable to waste water treatment in the environment-friendly industry.
Description
Technical field
The present invention relates to a kind of environmental friendliness, pollution-free, nontoxic starch/bentonite composite material preparation method and application.
Background technology
China's bentonite resource is abundant, and Regional Distribution is wide, and the prediction resource reserve ranks first in the world more than 8,000,000,000 tons; Proved reserves are 24.6 hundred million tons, account for 60% of the world.Bentonite belongs to the layer aluminosilicate clay mineral, be exploitation both at home and abroad the earliest, use one of the widest nonmetallic mineral, have the title of " omnipotent clay ".Bentonite has excellent physical and chemical performances such as cation exchange property, imbibition property, thixotropy, dispersion suspension property, adsorptivity, caking property and plasticity, low diffusivity, hypotonicity, chemical stability, heat endurance, is widely used in fields such as environmental protection, pharmaceutic adjuvant, catalyst and carrier, oil, casting, metallurgy, building, agricultural, animal husbandry, cosmetics of everyday use.
Bentonite is cheap, reserves are abundant, adsorption capacity is big, advantages of environment protection, is widely used as the basic material of sewage disposal adsorbent.Bentonite has characteristics such as special two-dimensional space structure, mineral surfaces suction-operated, interlayer cation exchange interaction, duct filtration and special nanostructured effect; Interlayer structure is controlled, surface nature can change; Activated, modification or composite modified processing can make multiple efficient bentonite base composite material.Common method of modifying has calcining modification, acid activation, organic intercalation, inorganic pillared and composite modified etc.
Organobentonite is that research is maximum a kind of, and it is with the montmorillonite organic double compound with montmorillonite (bentonitic main component) be combined into such as covalent bond, ionic bond, hydrogen bond, dipole effect and Van der Waals force by organic molecule, ion, polymer etc.Bentonite surface after organically-modified becomes hydrophobicity by hydrophily, and organic carbon content improves greatly, and some performance can compare favourably with active carbon.Therefore, organobentonite is the environmentally conscious materials of one type of superior performance, has a good application prospect.But organic modifiers commonly used like quaternary surfactant, macromolecule emulsion etc., is difficult to by natural degradation, and production cost is higher relatively simultaneously, and part has limited its extensive use.Therefore, preparation bentonite composite material efficient, cheap, nontoxic, that be prone to degraded is imperative.
The polysaccharide carbohydrate that starch is made up of glucose, amyloid crops have wheat, potato, cassava, sweet potato etc., and corn is the main source of producing starch.Native starch is of many uses, but the performance requirement that its cold water is insoluble, stick with paste that liquid is unstable, the transparency is poor, gel force is low, anti-mechanical agitation property and defectives such as stability is not enough, shortage resistance to water and emulsifying capacity can not satisfy modern industry production.So people utilize physics, chemistry or bioanalysis to handle starch, can obtain different converted starches through different method of modifying.Common chemical modification method has acidolysis, etherificate, hydroformylation, graft copolymerization etc., and the physical modification method mainly contains preparatory gelatinization, humid heat treatment, mechanical lapping processing etc., and the biological degeneration method mainly contains enzymolysis etc.Cationic starch is in starch, to introduce one type of widely used starch derivatives that cation group obtains through reactions such as etherificate, esterification or graft copolymerizations.
Starch resource is abundant, biodegradable; And can make it to become the multiple converted starch of excellent performance through structural modification; Be bentonite modified desirable feedstock, be expected to replace organic modified bentonite commonly used at present, for the preparation and the application of bentonite base composite material provides a kind of new thinking.
Summary of the invention
The purpose of this invention is to provide a kind of environmentally friendly starch/bentonite composite material preparation method, concrete steps as:
(1) Purification of Bentonite: take by weighing calcium-base bentonite, add in the distilled water, stir, standing demix discards the particle of bottom greater than 2 μ m, and it is subsequent use to get the upper strata bentonite suspension;
(2) bentonite sodium: add NaCl solution in the bentonite suspension that in step (1), obtains, stir 24h, behind the standing demix, abandoning supernatant; Add NaCl solution again, carry out the secondary sodium, stir standing demix, abandoning supernatant; Gained solid bentonite sample through centrifugal, washing, dry, grinding, is crossed 100 mesh sieves, be sodium-ionized bentonite;
(3) starch solution preparation: cationic starch is added in the distilled water, and furnishing 4% starch slurry after stirring, is warming up to 95 ℃, and insulation 20min adds the cold water dilution, regulates pH, and 60 ℃ of insulations are subsequent use;
(4) starch/bentonite composite material preparation: step (2) gained sodium-ionized bentonite is dispersed in the distilled water, adds the cationic starch aqueous solution, after stirred in water bath, to the product Separation of Solid and Liquid, washing; The gained solid sample is at 80 ℃ of oven dry down, 105 ℃ of following activation 1.0h; Grind, cross 100 mesh sieves, obtain starch/bentonite composite material.
Step (1) is raw materials used to be calcium-base bentonite, and its granularity is 200～300 orders.
The used sodium agent of step (2) is NaCl, and solution concentration is 0.50～1.0mol/L.
Step (3) is raw materials used to be cationic starch, and its cationic degree is 0.03～0.35, and the cationic starch concentration after the cold water dilution is 1～8g/L, and regulating pH is 5.0～8.0.
Sodium bentonite and starch solution mass ratio are 1: 4～8 in the step (4), and bath temperature is 25～75 ℃, and mixing time is 0.5～2.5 hour, and the content of starch of gained starch/bentonite composite material is 38.89～99.29mg/g.
Starch/the bentonite composite material of preparation is joined in the waste water that contains methylene blue, Congo red, p-nitrophenol and Cr (VI), on constant temperature oscillator, vibrate, realize removal these pollutants in the water.
A kind of environmentally friendly starch/bentonite composite material preparation method and application, the advantage and the characteristics of its embodiment are:
(1) the present invention is with natural, nontoxic converted starch---and cationic starch is that raw material carries out modification to bentonite, preparation starch/bentonite composite material, price is low, performance good, environmentally friendly, is fit to the environmental protection industry (epi) wastewater treatment;
(2) compare with the natural calcium base bentonite, variation has all taken place for the surface topography of gained starch/bentonite composite material, electronic characteristic and interlamellar spacing: specific area is by 33.96m
2/ g is increased to 57.76m
2/ g, Zeta potential is elevated to-13.01mV by-24.01mV, and interlamellar spacing increases to 1.515nm by 1.244nm.Utilize TEM analysis, scanning electron microscope analysis, infrared spectrum, thermogravimetric-differential thermal analysis etc. that its structure is characterized; Limellar stripping appears in proof novel cation starch/bentonite composite adsorbing material; The success of starch intercalation, its flocculating property improves, and surface hydrophobic strengthens.The absorption stability experiment proves that prepared product desorption rate is low, and stability is high.
(3) starch/bentonite composite material shows that to dyestuff methylene blue in the water and Congo red, p-nitrophenol and heavy metal ion Cr pollutant adsorption experiments such as (VI) starch/bentonite composite material that under optimum condition, prepares reaches more than 80% the removal effect of above-mentioned pollutant.
Description of drawings
Accompanying drawing 1 is the X-ray diffraction spectrogram of starch/bentonite composite material of the present invention;
Accompanying drawing 2 is stereoscan photographs of starch/bentonite composite material of the present invention;
Accompanying drawing 3 is infrared spectrograms of starch/bentonite composite material of the present invention.
The specific embodiment
Embodiment 1:
(1) taking by weighing the 100g granularity is 200 purpose calcium-base bentonites, adds 1.0L distilled water, stirs 2h, and standing demix discards the particle of bottom greater than 2 μ m, and it is subsequent use to get the upper strata bentonite suspension;
(2) sodium: in bentonite solution, add 0.50mol/LNaCl solution 2.5L, stir 24h, behind the standing demix, abandoning supernatant; Add 0.50mol/L NaCl solution 2.5L again, carry out the secondary sodium, stir 12h, standing demix, abandoning supernatant; Bentonite suspension with the centrifugal 20min of 8000rpm speed, is outwelled supernatant, add distilled water, repeated washing does not have (to use AgNO till the Cl-in supernatant
3Solution check Cl-); With the sample after the washing 80 ℃ down dry, pulverize is crossed 100 mesh sieves, is the bentonite after the purification sodium;
(3) preparation starch solution: with cationic degree is that 0.3 cationic starch adds in the distilled water, and furnishing 4% starch slurry stirs, and is warming up to 95 ℃, and insulation 20min adds cold water and is diluted to 7g/L, and it is subsequent use to regulate 7.0,60 ℃ of insulations of pH;
(4) preparation starch/bentonite composite material: the bentonite of above-mentioned purification sodium is dispersed in the distilled water; According to sodium bentonite and starch solution mass ratio is that 1: 5 ratio quantitatively adds the cationic starch aqueous solution; In temperature is that 60 ℃ of stirred in water bath are after 2 hours, to the product Separation of Solid and Liquid; The gained solid sample is at 80 ℃ of oven dry down, 105 ℃ of following activation 1.0h; Grind, cross 100 mesh sieves, obtain starch/bentonite composite material.
The content of starch of the starch/bentonite composite material that obtains according to above-mentioned steps is 99.29mg/g, and specific area is 57.76m
2/ g, Zeta potential-13.01mV, interlamellar spacing d
001Be 1.515nm, X ray spectrogram, stereoscan photograph and infrared spectrogram are respectively shown in accompanying drawing 1-3.
The methylene blue dye solution 25mL that pipettes 200mg/L places conical flask, the 150min that on oscillator, vibrates behind adding 0.07g starch/bentonite composite material, and the clearance of methylene blue dye is 99.3%.
The Congo red dye solution 25mL that pipettes 100mg/L places conical flask, the 120min that on oscillator, vibrates behind adding 0.035g starch/bentonite composite material, and the clearance of Congo red dyestuff is 96.7%.
The p-nitrophenyl phenol solution 25mL that pipettes 100mg/L places conical flask, the 30min that on oscillator, vibrates behind adding 0.07g starch/bentonite composite material, and the clearance of p-nitrophenol is 80.4%.
Cr (VI) the solution 25mL that pipettes 5.0mg/L places conical flask, the 45min that on oscillator, vibrates behind adding 0.11g starch/bentonite composite material, and the clearance of Cr (VI) is 95.5%.
Embodiment 2～6:
Implementation method is identical with embodiment 1; Change the granularity of calcium-base bentonite in the step (1); NaCl solution concentration in the step (2); Cationic degree, concentration, the pH value of solution of cationic starch in the step (3), sodium bentonite and starch solution mass ratio, bath temperature, mixing time in the step (4), the content of starch of gained starch/bentonite composite material, Zeta potential and interlamellar spacing d
001And it is as shown in the table to the clearance of dyestuff methylene blue in the water, Congo red and p-nitrophenol, Cr (VI).
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Calcium-base bentonite granularity (order) | 300 | 200 | 200 | 200 | 200 |
| NaCl solution concentration (mol/L) | 1.0 | 1.0 | 0.8 | 0.5 | 0.5 |
| The cationic degree of cationic starch | 0.03 | 0.1 | 0.3 | 0.35 | 0.3 |
| Cationic starch concentration (g/L) | 1.0 | 1.0 | 5.0 | 3.0 | 8.0 |
| Cationic starch solution pH | 8.0 | 5.0 | 6.0 | 5.0 | 7.0 |
| Sodium bentonite and starch solution mass ratio | 1∶4 | 1∶8 | 1∶5 | 1∶6 | 1∶5 |
| Bath temperature (℃) | 75 | 25 | 40 | 60 | 60 |
| Mixing time (h) | 2.5 | 0.5 | 2.5 | 1 | 2 |
| The content of starch of composite (mg/g) | 38.89 | 45.31 | 69.85 | 78.66 | 87.22 |
| Zeta potential (mV) | -19.07 | -16.09 | -19.07 | -17.58 | -17.77 |
| Interlamellar spacing d 001(nm) | 1.494 | 1.461 | 1.505 | 1.505 | 1.473 |
| The clearance of methylene blue dye (%) | 50.6 | 60.9 | 76.4 | 82.3 | 90.2 |
| The clearance of Congo red dyestuff (%) | 54.5 | 63.8 | 75.4 | 79.9 | 91.2 |
| The clearance of p-nitrophenol (%) | 48.8 | 52.3 | 59.5 | 70.3 | 78.7 |
| The clearance (%) of Cr (VI) | 64.5 | 69.8 | 77.7 | 82.9 | 89.5 |
Claims (6)
1. the preparation method of an environmentally friendly starch/bentonite composite material is characterized in that comprising being prepared as follows step:
(1) Purification of Bentonite: take by weighing calcium-base bentonite, add in the distilled water, stir, standing demix discards the particle of bottom greater than 2 μ m, and it is subsequent use to get the upper strata bentonite suspension;
(2) bentonite sodium: add NaCl solution in the bentonite suspension that in step (1), obtains, stir 24h, behind the standing demix, abandoning supernatant; Add NaCl solution again, carry out the secondary sodium, stir standing demix, abandoning supernatant; Gained solid bentonite sample through centrifugal, washing, dry, grinding, is crossed 100 mesh sieves, be sodium-ionized bentonite;
(3) starch solution preparation: cationic starch is added in the distilled water, and furnishing 4% starch slurry after stirring, is warming up to 95 ℃, and insulation 20min adds the cold water dilution, regulates pH, and 60 ℃ of insulations are subsequent use;
(4) starch/bentonite composite material preparation: step (2) gained sodium-ionized bentonite is dispersed in the distilled water, adds the cationic starch aqueous solution, after stirred in water bath, to the product Separation of Solid and Liquid, washing; The gained solid sample is at 80 ℃ of oven dry down, 105 ℃ of following activation 1.0h; Grind, cross 100 mesh sieves, obtain starch/bentonite composite material.
2. the preparation method of a kind of environmentally friendly starch/bentonite composite material according to claim 1 is characterized in that step (1) is raw materials used and is calcium-base bentonite that its granularity is 200～300 orders.
3. the preparation method of a kind of environmentally friendly starch/bentonite composite material according to claim 1 is characterized in that the used sodium agent of step (2) is NaCl, and solution concentration is 0.50～1.0mol/L.
4. the preparation method of a kind of environmentally friendly starch/bentonite composite material according to claim 1; It is characterized in that step (3) is raw materials used for cationic starch; Its cationic degree is 0.03～0.35; Cationic starch concentration after the cold water dilution is 1～8g/L, and regulating pH is 5.0～8.0.
5. the preparation method of a kind of environmentally friendly starch/bentonite composite material according to claim 1; It is characterized in that middle sodium bentonite of step (4) and starch solution mass ratio are 1: 4～8; Bath temperature is 25～75 ℃; Mixing time is 0.5～2.5 hour, and the content of starch of gained starch/bentonite composite material is 38.89～99.29mg/g.
6. the application of the said environmentally friendly starch/bentonite composite material that obtains according to the as above arbitrary preparation method of claim 1-5; It is characterized in that the starch/bentonite composite material of preparation is joined in the waste water that contains methylene blue, Congo red, p-nitrophenol and Cr (VI); On constant temperature oscillator, vibrate, realize removal these pollutants in the water.
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| CN103432999A (en) * | 2013-08-21 | 2013-12-11 | 太仓碧奇新材料研发有限公司 | Preparation method of rice-straw based chromium ion adsorbing material |
| CN105032365A (en) * | 2015-07-06 | 2015-11-11 | 安徽成方新材料科技有限公司 | Composite spherical active carbon with electrostatic adsorption effect, and preparation method thereof |
| CN105293511A (en) * | 2015-11-30 | 2016-02-03 | 浙江丰虹新材料股份有限公司 | Easy-to-disperse sodium bentonite and preparation method thereof |
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| CN107162143A (en) * | 2017-07-01 | 2017-09-15 | 辽东学院 | Dyeing waste water purifies flocculant and its dyeing waste water purification applications |
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| CN110038539A (en) * | 2019-04-23 | 2019-07-23 | 襄阳先创环保科技有限公司 | A kind of preparation method of the garbage leachate wastewater inorganic agent based on montmorillonite |
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| CN110756159A (en) * | 2019-11-06 | 2020-02-07 | 中山职业技术学院 | Preparation method of high-performance modified sodium bentonite nano composite adsorption material |
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