CN104492387A - Method for producing modified bentonite by using urea-chitosan - Google Patents
Method for producing modified bentonite by using urea-chitosan Download PDFInfo
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- CN104492387A CN104492387A CN201410665818.5A CN201410665818A CN104492387A CN 104492387 A CN104492387 A CN 104492387A CN 201410665818 A CN201410665818 A CN 201410665818A CN 104492387 A CN104492387 A CN 104492387A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
Abstract
The invention discloses a method for producing modified bentonite by using urea-chitosan, which includes the following steps: on a weight basis, adding 1-5 parts of urea into 40-60 parts of bentonite, mixing and grinding, adding 400-700 parts of water to obtain a bentonite suspension; on a weight basis, dissolving 3-7 parts of chitosan into an acetic acid solution with a mass fraction of 1.0-3.0% to obtain a chitosan acetic acid solution with a chitosan mass fraction of 1.0-2.0%; dropwise adding the chitosan acetic acid solution into the bentonite suspension in a water bath, water-bathing for 2-3h, cooling and filtering, washing a filter cake with water, drying, grinding and sieving the filter cake to obtain the modified bentonite. The inventive method has the advantages of simple process and low production condition requirements; and the resulting adsorbent has obvious removal effect in acidic condition, the production process is convenient and feasible, and has good application prospects.
Description
Technical field
The present invention relates to the preparation field of modified alta-mud, specifically one utilizes urea-shitosan to produce method for preparation of modified bentonite.
Background technology
The technology of current improvement mine tailing heavy metal pollution has following several: neutralisation, bactericide method, covering isolation method and passivation coating method, and wherein spray fixative process mine tailing cost lower, operation more for convenience.Find the important step that the high fixative of cost performance is process mine tailing, phosphate and hydroxyapatite are the fixatives relatively commonly used, but it is expensive, and phosphorus may be caused to pollute, and make it apply and are restricted.
Bentonitic main component is montmorillonite, has certain adsorption capacity, at China's rich reserves, cheap, and rationally modified have larger application potential.The adsorption effect of modified bentonite heavy metal is obviously better than original soil, but have that cost of manufacture is high, complex manufacturing technology and the problem such as comprehensive treatment effect is poor, therefore the selection of modifier and the optimization of modified technique are important research topics.
Hechi prefecture of Guangxi has a large amount of Tailings Dam, is mostly that utilizing mountain valley to build a dam banks up, and lacks seepage control measure.The annual half rainfall in this area is acid rain, and acid rain mean ph value is 4.6.Under the long period of soaking of acid rain, constantly there is the physical-chemical reactions such as ion-exchange, corrosion dissolving, mass transfer and migration in mine tailing and water chemistry solution, heavy metal element possibility polluted surface water, the underground water and soil of leaching, thus be detrimental to health.Therefore, that to study under acid rain condition heavy metal element in mine tailing is fixed with very important meaning.
Summary of the invention
Technical problem to be solved by this invention is, the problem of additional pollution and high cost can be brought for traditional fixative process heavy metal pollution, simultaneously under acid condition to the treatment effect of mine tailing heavy metal, there is provided one to utilize urea-shitosan to produce method for preparation of modified bentonite, make the modified alta-mud of gained modified effect in acid condition better.
The present invention solves the problems of the technologies described above taked technical scheme:
One utilizes urea-shitosan to produce method for preparation of modified bentonite, comprises following concrete steps:
(1) count by weight, take 1 ~ 5 part of urea and join agitation grinding in 40 ~ 60 parts of bentonites, add water 400 ~ 700 parts and make medicinal bentonite suspension;
(2) count by weight, take 3 ~ 7 parts of shitosans, adding mass fraction is dissolve in the acetum of 1.0 ~ 3.0%, and the mass fraction obtaining shitosan is the chitosan-acetic acid solution of 1.0% ~ 2.0%.
(3) count by weight, lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 70 ~ 90 DEG C of water-baths, water-bath 2 ~ 3h at the temperature of 70 ~ 90 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 3 ~ 6 times, dries 20 ~ 24h by gained filter cake in 70 ~ 90 DEG C of baking ovens; Then grind, sieve, obtain modified alta-mud.
Sieving described in step (3) referred to 200 mesh sieves.
Compared with prior art, beneficial effect of the present invention is:
Urea and shitosan is adopted to carry out bentonitic original soil composite modified, method of operating is less demanding to working condition, manufacturing process facilitates feasible, the modified alta-mud removal effect of gained is obvious, be low to moderate the acid condition of 4.5 in pH value under, modified alta-mud has good fixed effect to the Zn in certain tin ore mine tailing, has good application prospect.
Accompanying drawing explanation
Fig. 1 is that the different modified alta-mud dosage of the embodiment of the present invention 1 is on the impact of Zn fixed rate.
Fig. 2 is that after the embodiment of the present invention 1 1.5g bentonite in treatment mine tailing, solution acidity is on the impact of Zn fixed rate.
Fig. 3 be in the embodiment of the present invention 1 different temperatures on the impact of Zn fixed rate.
Fig. 4 is that after the embodiment of the present invention 1 1.5g bentonite in treatment mine tailing, extraction time is on the impact of Zn fixed rate.
Fig. 5 is the surface texture adopting electron-microscope scanning (SEM) to analyze original soil in the embodiment of the present invention 1, and multiplication factor is 10000 times.
Fig. 6 is the surface texture adopting electron-microscope scanning (SEM) to analyze modified alta-mud in the embodiment of the present invention 1, and multiplication factor is 10000 times.
Fig. 7 is the infrared spectrum analysis figure of original soil in the embodiment of the present invention 1.
Fig. 8 is the infrared spectrum analysis figure of modified alta-mud in the embodiment of the present invention 1.
Fig. 9 is the X diffracting spectrum of original soil and modified alta-mud in the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment and accompanying drawing, technical scheme of the present invention and technique effect are described further.
Embodiment 1
One utilizes urea-shitosan to produce method for preparation of modified bentonite, comprises following concrete steps:
(1) take 2g urea and join agitation grinding in 50g bentonite, the 500g that adds water makes medicinal bentonite suspension;
(2) take 5g shitosan, adding 500ml mass fraction is dissolve in the acetum of 1.0 ~ 3.0%, obtains chitosan-acetic acid solution.
(3) lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 80 DEG C of water-baths, continue water-bath 2h at the temperature of 80 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 5 times, dries 24h by gained filter cake in 80 DEG C of baking ovens; Then grind, cross 200 mesh sieves, obtain modified alta-mud.
1. the modified alta-mud of original soil and embodiment 1 gained is to the contrast test of the fixed rate of zinc in mine tailing:
Take original soil as contrast, the modified alta-mud of embodiment 1 gained is used for fixing the zinc in mine tailing, be taken at that pH is 4.0, under normal temperature condition, extraction time is 12 hours, and different dosage is fixed the zinc in 50g mine tailing, and measurement result as shown in Figure 1; Being taken at dosage is under 1.5g, normal temperature condition, and extraction time is 12 hours, is fixed under condition of different pH to the zinc in 50g mine tailing, and measurement result as shown in Figure 2; To be taken at dosage be 1.5g, pH is under 4.0 conditions, and extraction time is 12 hours, is fixed under condition of different temperatures to the zinc in 50 mine tailings, and measurement result as shown in Figure 3; To be taken at dosage be 1.5g, pH is 4.0, under room temperature condition, be fixed the zinc in 50g mine tailing under different extraction time, measurement result as shown in Figure 4.From the result of Fig. 1-Fig. 4, compared with original soil, under the same conditions, the modified alta-mud of embodiment 1 gained can significantly improve the fixed rate of zinc in mine tailing.
2. the SEM comparative analysis of the modified alta-mud of original soil and embodiment 1 gained:
Adopt the surface texture of the modified alta-mud of sem analysis original soil and embodiment 1 gained, multiplication factor is 10000 times.The results are shown in Figure 5 and Fig. 6, comparison diagram 5 and Fig. 6 known, the smooth surface of original soil and closely knit, modified alta-mud surface is more aobvious fluffy, and modifier urea and chitosan loaded bentonite surface of having arrived are described, the performance of gained modified alta-mud is better than original soil.
3. the infrared spectrum comparative analysis of the modified alta-mud of original soil and embodiment 1 gained
Analyze with the modified alta-mud of infrared spectrometric analyzer to original soil and embodiment 1 gained, result as shown in Figure 7 and Figure 8.From Fig. 7 and Fig. 8, modified alta-mud is at wave number 1384.75cm
-1having there is acid amides vibration absorption peak in place, illustrates that urea there occurs reaction with original soil and becomes modified alta-mud.
4. the XRD comparative analysis of the modified alta-mud of original soil and embodiment 1 gained:
In order to verify that urea and shitosan are inserted between bentonite bed further, instead of simply mix.The interlayer structure of original soil and modified alta-mud with XRD analysis, X diffracting spectrum is as shown in Figure 9.As can be seen from Figure 9, the d001 peak of modified alta-mud moves to left relative to original soil, and 2 θ of its correspondence are 4.94o.According to formula 2dsin θ=λ, the interlamellar spacing d that can calculate modified alta-mud is 1.79nm, and the interlamellar spacing of original soil is 1.57nm.Modified alta-mud interlamellar spacing is greater than original soil, proves urea and chitosan intercalation success, optimizes the performance of original soil.
Embodiment 2
One utilizes urea-shitosan to produce method for preparation of modified bentonite, comprises following concrete steps:
(1) take 1g urea and join agitation grinding in 40g bentonite, the 400ml that adds water makes medicinal bentonite suspension;
(2) take 4.5g shitosan, adding 400ml mass fraction is dissolve in the acetum of 1.0%, obtains chitosan-acetic acid solution.
(3) lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 70 DEG C of water-baths, continue water-bath 2h at the temperature of 70 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 3 times, dries 24h by gained filter cake in 70 DEG C of baking ovens; Then grind, cross 200 mesh sieves, obtain modified alta-mud.
Embodiment 3
One utilizes urea-shitosan to produce method for preparation of modified bentonite, comprises following concrete steps:
(1) take 3g urea and join agitation grinding in 55g bentonite, the 550ml part that adds water makes medicinal bentonite suspension;
(2) take 6.0g shitosan, adding 550ml mass fraction is dissolve in the acetum of 2.5%, obtains chitosan-acetic acid solution.
(3) lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 85 DEG C of water-baths, continue water-bath 2.5h at the temperature of 85 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 6 times, dries 20h by gained filter cake in 85 DEG C of baking ovens; Then grind, cross 200 mesh sieves, obtain modified alta-mud.
Embodiment 4
One utilizes urea-shitosan to produce method for preparation of modified bentonite, comprises following concrete steps:
(1) take 5g urea and join agitation grinding in 60g bentonite, the 650ml that adds water makes medicinal bentonite suspension;
(2) take 7g shitosan, adding 700ml mass fraction is dissolve in the acetum of 3.0%, obtains chitosan-acetic acid solution.
(3) lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 90 DEG C of water-baths, continue water-bath 2h at the temperature of 90 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 4 times, dries 22h by gained filter cake in 90 DEG C of baking ovens; Then grind, cross 200 mesh sieves, obtain modified alta-mud.
Claims (2)
1. utilize urea-shitosan to produce a method for preparation of modified bentonite, it is characterized in that, comprise following concrete steps:
(1) count by weight, take 1 ~ 5 part of urea and join agitation grinding in 40 ~ 60 parts of bentonites, add water 400 ~ 700 parts and make medicinal bentonite suspension;
(2) count by weight, take 3 ~ 7 parts of shitosans, adding mass fraction is dissolve in the acetum of 1.0 ~ 3.0%, and the mass fraction obtaining shitosan is the chitosan-acetic acid solution of 1.0% ~ 2.0%;
(3) count by weight, lentamente the chitosan-acetic acid solution that step (2) obtains is added drop-wise in the medicinal bentonite suspension that step (1) obtains in 70 ~ 90 DEG C of water-baths, water-bath 2 ~ 3h at the temperature of 70 ~ 90 DEG C, after water-bath terminates, be cooled to room temperature, filter, washing filter cake 3 ~ 6 times, dries 20 ~ 24h by gained filter cake in 70 ~ 90 DEG C of baking ovens; Then grind, sieve, obtain modified alta-mud.
2. method for preparation of modified bentonite produced by the urea-shitosan that utilizes according to claim 1, and it is characterized in that, sieving described in step (3) referred to 200 mesh sieves.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376849A (en) * | 2017-08-09 | 2017-11-24 | 河海大学 | A kind of application of ethylenediamine tetraacetic acid modified diatomite adsorbant and preparation method thereof and processing heavy metal ions in wastewater |
| CN108771061A (en) * | 2018-03-30 | 2018-11-09 | 重庆火吉健康产业（集团）有限公司 | Rocket ram jet concentration stock solution with anticancer function and preparation method thereof |
| CN110548490A (en) * | 2018-05-31 | 2019-12-10 | 华中科技大学 | Preparation method and application of recyclable lanthanum modified bentonite phosphorus removal material |
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| CN101058426A (en) * | 2007-04-13 | 2007-10-24 | 沈阳化工学院 | Environment-friendly modified bentonite and preparation method thereof |
| US20090167993A1 (en) * | 2007-12-31 | 2009-07-02 | Industrial Technology Research Institute | Method for forming optical compensating films, optical compensating films formed thereby, structure of optical compensating films, and polarizing plates |
| CN101734677A (en) * | 2008-11-05 | 2010-06-16 | 北京化工大学 | Method for stripping laminated inorganic material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058426A (en) * | 2007-04-13 | 2007-10-24 | 沈阳化工学院 | Environment-friendly modified bentonite and preparation method thereof |
| US20090167993A1 (en) * | 2007-12-31 | 2009-07-02 | Industrial Technology Research Institute | Method for forming optical compensating films, optical compensating films formed thereby, structure of optical compensating films, and polarizing plates |
| CN101734677A (en) * | 2008-11-05 | 2010-06-16 | 北京化工大学 | Method for stripping laminated inorganic material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376849A (en) * | 2017-08-09 | 2017-11-24 | 河海大学 | A kind of application of ethylenediamine tetraacetic acid modified diatomite adsorbant and preparation method thereof and processing heavy metal ions in wastewater |
| CN107376849B (en) * | 2017-08-09 | 2020-07-31 | 河海大学 | Ethylene diamine tetraacetic acid modified diatomite adsorbent, preparation method thereof and application of adsorbent in treatment of heavy metal ions in wastewater |
| CN108771061A (en) * | 2018-03-30 | 2018-11-09 | 重庆火吉健康产业（集团）有限公司 | Rocket ram jet concentration stock solution with anticancer function and preparation method thereof |
| CN110548490A (en) * | 2018-05-31 | 2019-12-10 | 华中科技大学 | Preparation method and application of recyclable lanthanum modified bentonite phosphorus removal material |
| CN110548490B (en) * | 2018-05-31 | 2020-10-30 | 华中科技大学 | Preparation method and application of recyclable lanthanum modified bentonite phosphorus removal material |
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