CN101428809A - Method for nano-attapulgite stone clay grain surface magnetization modification - Google Patents
Method for nano-attapulgite stone clay grain surface magnetization modification Download PDFInfo
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- CN101428809A CN101428809A CNA2008102447090A CN200810244709A CN101428809A CN 101428809 A CN101428809 A CN 101428809A CN A2008102447090 A CNA2008102447090 A CN A2008102447090A CN 200810244709 A CN200810244709 A CN 200810244709A CN 101428809 A CN101428809 A CN 101428809A
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Abstract
A method for nanometer attapulgite clay particle surface magnetized modification is characterized in that an attapulgite clay solution with the pH value being 3-10 is prepared, stirred and heated, an FeCl2 solution is added drop by drop at 30-100 DEG C, a KOH or NaOH solution is added drop by drop at the same time for keeping the pH value of the solution, and the temperature for solution reaction keeps constant; after FeCl2 is added drop by drop, stirring is performed continuously and the temperature is kept for 30-60 minutes at the same time, and then a reaction solution is obtained; the reaction solution is cleaned by ionized water, attapulgite clay particles are obtained after filtration and aired at the room temperature, and the magnetized anometer attapulgite clay particles can be obtained. The invention can be utilized to obtain nanometer attapulgite clay particles with surface magnetic particles on the basis of simple operation.
Description
Technical field
The present invention relates to the attapulgite stone clay grain surface magnetization modification method,, bring more potential application by making attapulgite stone clay grain surface magnetization.
Background technology
Attapulgite be a kind of layer of chain-like structure contain Shuifu County's zeopan clay mineral, have natural nanofiber characteristic, specific surface area is big, selects adsorptivity strong; Have very strong cationic exchange and adsorption bleaching characteristic; And can be used as catalyzer and support of the catalyst; Thixotropy is good, and effect such as tool sterilization, deodorizing, detoxification, desinsection.All be widely used at aspects such as oil, chemical industry, building materials, papermaking, medicine, agriculturals.
But in use, dispersive attapulgite clay particulate separates or concentration ratio difficulty in solution, and if we carry out suitable magnetized surface modification to it, then this problem can be readily solved; Aspect pharmacology, the nano-attapulgite stone after the magnetization all has potential to use in drug conveying or medical imaging, even is expected to become the carrier of targeted drug in addition.Yet so far, relevant nano-attapulgite stone particulate magnetized surface but is not reported.
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, a kind of method of nano-attapulgite stone clay grain surface magnetization modification is provided, make its surface magnetization, thereby makes it can bring more potential application.
The characteristics of the inventive method are to operate according to the following procedure:
1, the method for nano-attapulgite stone clay grain surface magnetization modification is characterized in that operating as follows:
A, preparation attapulgite clay solution, volume parts is 4, and strength of solution is 1-20g/L, and the pH value is 3-10;
B, stirring attapulgite clay solution, heating when temperature reaches 30-100 ℃, dropwise splashes into FeCl simultaneously
2Solution, described FeCl
2Strength of solution is 0.1-2.0mol/l, and volume parts is 0.5-2; Dropwise add simultaneously KOH or NaOH solution, to keep the pH value of solution value constant, the solution reaction temperature remains constant; Work as FeCl
2After dropwising, continue to stir stop after being incubated 30-60 minute simultaneously reaction soln;
C, after reaction soln is cleaned with ionized water, filter the attapulgite clay particle, place air drying at ambient temperature, promptly get magnetized nano-attapulgite stone clay particle.
2, the method for nano-attapulgite stone clay grain surface magnetization modification according to claim 1 is characterized in that adding in reaction soln for the cleaning of reaction soln in the described step 2 distilled water of capacity, filters flush away Cl soluble in water then
-, K
+Or Na
+, filter the gained pressed powder and be attapulgite clay.
In the inventive method, divalence Fe ion and oxygen reaction generate Fe
3O
4Be deposited on nanometer concave-convex rod particle on, thereby make Attapulgite surface magnetization modification.Attapulgite behind the magnetization modification is carried out the material analysis test, find nanometer Fe
3O
4Particle is grown on attapulgite, material and tool soft magnetic property.
Compared with the prior art, beneficial effect of the present invention is embodied in:
Utilize the present invention, on the simple operations basis, can obtain surface magnetism particulate Attapulgite nano particle, the Attapulgite through magnetization modification can be applied in every field such as oil, chemical industry, medicine, agricultural more widely.
Description of drawings
Fig. 1 is the transmission electron microscope photo of commercially available attapulgite.
Fig. 2, Fig. 3 and Fig. 4 are respectively the transmission electron microscope photo of embodiment 1,2,3 products that obtain
Fig. 5 by embodiment 3 the magnetzation curve of acquisition product.
Below the invention will be further described by embodiment.
Embodiment
Embodiment 1:
Get the Attapulgite solution 100ml of 6g/L, be heated 80 ℃ and stir; Subsequently, with FeCl
2Solution 25mL, 0.2mol/L add in the Attapulgite solution with the speed of 5mL/min, dropwise add KOH solution simultaneously, keep pH value of solution=5.
After reaction finishes, reaction soln is filtered cleaning 3 times with ionized water, filter gained attapulgite clay particle and place the air at room temperature drying.
Attapulgite behind the magnetization modification is observed, found that the Attapulgite clay particle is not by Fe under the present embodiment
3O
4Particle covers fully, as shown in Figure 2.
Embodiment 2:
Get the Attapulgite solution 100ml of 12g/L, be heated 60 ℃ and stir; Subsequently, with FeCl
2Solution 25mL, 0.9mol/L add in the Attapulgite solution with the speed of 5mL/min, dropwise add KOH solution simultaneously, keep pH value of solution=8.
After reaction finishes, reaction soln is filtered cleaning 3 times with ionized water, filter gained attapulgite clay particle and place the air at room temperature drying.
Attapulgite behind the magnetization modification is observed, found that the Attapulgite clay particle is almost completely by Fe under the present embodiment
3O
4The particle parcel, as shown in Figure 3.
Embodiment 3:
Get the Attapulgite solution 100ml of 18g/L, be heated 80 ℃ and stir; Subsequently, with FeCl
2Solution 25mL, 1.4mol/L add beaker with the speed of 5mL/min, dropwise add KOH solution simultaneously, keep pH value of solution=8.
After reaction finishes, reaction soln is filtered cleaning 3 times with ionized water, filter gained attapulgite clay particle and place the air at room temperature drying.
Attapulgite behind the magnetization modification is observed, found that the Attapulgite clay particle is by Fe under the present embodiment
3O
4Particle wraps up fully, and Fe
3O
4Particle is looked bigger, and the magnetzation curve of the product that obtains as shown in Figure 4.
Claims (2)
1, the method for nano-attapulgite stone clay grain surface magnetization modification is characterized in that operating as follows:
A, preparation attapulgite clay solution, volume parts is 4, and strength of solution is 1-20g/L, and the pH value is 3-10;
B, stirring attapulgite clay solution, heating when temperature reaches 30-100 ℃, dropwise splashes into FeCl simultaneously
2Solution, described FeCl
2Strength of solution is 0.1-2.0mol/l, and volume parts is 0.5-2; Dropwise add simultaneously KOH or NaOH solution, to keep the pH value of solution value constant, the solution reaction temperature remains constant; Work as FeCl
2After dropwising, continue to stir stop after being incubated 30-60 minute simultaneously reaction soln;
C, after reaction soln is cleaned with ionized water, filter the attapulgite clay particle, place air drying at ambient temperature, promptly get magnetized nano-attapulgite stone clay particle.
2, the method for nano-attapulgite stone clay grain surface magnetization modification according to claim 1 is characterized in that adding in reaction soln for the cleaning of reaction soln in the described step 2 distilled water of capacity, filters flush away Cl soluble in water then
-, K
+Or Na
+, filter the gained pressed powder and be attapulgite clay.
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Cited By (12)
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CN102258978A (en) * | 2011-06-24 | 2011-11-30 | 淮阴师范学院 | Method for preparing nano Fe3O4 coated attapulgite magnetic composite adsorbent |
CN102389772A (en) * | 2011-09-30 | 2012-03-28 | 淮阴师范学院 | Method for preparing lipophilic magnetic attapulgite composite absorbent |
CN102649954A (en) * | 2012-05-17 | 2012-08-29 | 兰州大学 | Immobilized enzyme for magnetic nanometer clay carrier and regenerating method thereof |
CN103117149A (en) * | 2011-11-16 | 2013-05-22 | 核工业北京地质研究院 | Magnetization method of surface of quartz granule |
CN103230796A (en) * | 2013-04-25 | 2013-08-07 | 六安科瑞达新型材料有限公司 | Preparation method of attapulgite supported ferroferric oxide |
CN104058662A (en) * | 2014-06-13 | 2014-09-24 | 长江勘测规划设计研究有限责任公司 | Anti-seepage composite grouting material for underground nuclear power station and application of grouting material |
CN105772077A (en) * | 2016-03-17 | 2016-07-20 | 中国科学院广州能源研究所 | Magnetic attapulgite supported ionic liquid catalyst and preparation method thereof |
CN107051412A (en) * | 2017-05-24 | 2017-08-18 | 安徽工业大学 | A kind of preparation method of magnetic palygorskite nano composite material |
CN107473269A (en) * | 2017-07-26 | 2017-12-15 | 淮阴工学院 | The preparation method and application of ceria attapulgite ferroferric oxide magnetic nano composite |
CN108622908A (en) * | 2018-05-21 | 2018-10-09 | 东北大学 | A kind of method that clay alteration prepares pale yellow-reddish brown colour system mineral material |
CN112934170A (en) * | 2021-01-30 | 2021-06-11 | 上海师范大学 | Magnetic nano-ore composite material for efficiently removing thallium, and preparation method and application thereof |
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2008
- 2008-11-26 CN CN2008102447090A patent/CN101428809B/en not_active Expired - Fee Related
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CN102258978A (en) * | 2011-06-24 | 2011-11-30 | 淮阴师范学院 | Method for preparing nano Fe3O4 coated attapulgite magnetic composite adsorbent |
CN102258978B (en) * | 2011-06-24 | 2012-10-24 | 淮阴师范学院 | Method for preparing nano Fe3O4 coated attapulgite magnetic composite adsorbent |
CN102389772B (en) * | 2011-09-30 | 2012-11-21 | 淮阴师范学院 | Method for preparing lipophilic magnetic attapulgite composite absorbent |
CN102389772A (en) * | 2011-09-30 | 2012-03-28 | 淮阴师范学院 | Method for preparing lipophilic magnetic attapulgite composite absorbent |
CN103117149B (en) * | 2011-11-16 | 2015-07-15 | 核工业北京地质研究院 | Magnetization method of surface of quartz granule |
CN103117149A (en) * | 2011-11-16 | 2013-05-22 | 核工业北京地质研究院 | Magnetization method of surface of quartz granule |
CN102649954A (en) * | 2012-05-17 | 2012-08-29 | 兰州大学 | Immobilized enzyme for magnetic nanometer clay carrier and regenerating method thereof |
CN103230796A (en) * | 2013-04-25 | 2013-08-07 | 六安科瑞达新型材料有限公司 | Preparation method of attapulgite supported ferroferric oxide |
CN104058662A (en) * | 2014-06-13 | 2014-09-24 | 长江勘测规划设计研究有限责任公司 | Anti-seepage composite grouting material for underground nuclear power station and application of grouting material |
CN105772077A (en) * | 2016-03-17 | 2016-07-20 | 中国科学院广州能源研究所 | Magnetic attapulgite supported ionic liquid catalyst and preparation method thereof |
CN105772077B (en) * | 2016-03-17 | 2018-09-28 | 中国科学院广州能源研究所 | A kind of magnetism attapulgite loaded ionic-liquid catalyst and preparation method thereof |
CN107051412A (en) * | 2017-05-24 | 2017-08-18 | 安徽工业大学 | A kind of preparation method of magnetic palygorskite nano composite material |
CN107473269A (en) * | 2017-07-26 | 2017-12-15 | 淮阴工学院 | The preparation method and application of ceria attapulgite ferroferric oxide magnetic nano composite |
CN108622908A (en) * | 2018-05-21 | 2018-10-09 | 东北大学 | A kind of method that clay alteration prepares pale yellow-reddish brown colour system mineral material |
CN112934170A (en) * | 2021-01-30 | 2021-06-11 | 上海师范大学 | Magnetic nano-ore composite material for efficiently removing thallium, and preparation method and application thereof |
CN112980455A (en) * | 2021-03-05 | 2021-06-18 | 中国水稻研究所 | Preparation method of modified attapulgite water-retaining agent for saline-alkali soil |
CN112980455B (en) * | 2021-03-05 | 2021-10-22 | 中国水稻研究所 | Preparation method of modified attapulgite water-retaining agent for saline-alkali soil |
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