CN103601203A - Halloysite nanotube purification method - Google Patents
Halloysite nanotube purification method Download PDFInfo
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- CN103601203A CN103601203A CN201310513487.9A CN201310513487A CN103601203A CN 103601203 A CN103601203 A CN 103601203A CN 201310513487 A CN201310513487 A CN 201310513487A CN 103601203 A CN103601203 A CN 103601203A
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Abstract
The invention relates to a halloysite nanotube purification method. The method comprises the following steps: dissolving polyacrylamide in deionized water to obtain a flocculating agent solution; taking halloysite nanotube raw ore and water, stirring, breaking the halloysite raw ore, dispersing the obtained precipitate, taking a reducing agent and a dispersant, adding to the obtained halloysite raw ore dispersion, stirring, and filtering out impurities; diluting the obtained filtered mixed solution, adding the flocculating agent solution for flocculation, allowing the obtained solution to stand, filtering out the upper layer clear water, and cleaning the obtained flocculation product; and drying the product, grinding, and sieving by a 200 mesh filter sieve. The method has the following beneficial effects: (1) the adoption of the dispersed suspension precipitation method to purify precipitates impurities in halloysite, and the adoption of sodium hydrosulfite as a reducing agent removes metal oxides (such as iron oxide), so high-purity halloysite is obtained; (2) the purification efficiency is high, and 70% of the content of halloysite in the raw ore is reserved; and (3) the method is simple, fast, and feasible, is free from contamination, can realize the industrialized production, and provides the foundation for the utilization and research of the halloysite.
Description
Technical field
The invention belongs to field of inorganic materials, especially a kind of halloysite nanotubes method of purification rapidly and efficiently.
Background technology
Halloysite nanotubes (HNTs) is the cheap natural nano pipe of a kind of well-crystallized, and its molecular formula is Al
2si
2o
5(OH)
4nH
2o (n=0 or 2), normal is multi-walled pipes shape structure, by the dislocation that do not match of the space between alumina octahedral sheet and silicon-oxy tetrahedron layer, impel tabular crystal to be curled into pipe, pipe external diameter is 10～20nm, internal diameter is 40～100nm, length is 0.5～40 μ m, crystal layer number is 15～40, at least at one-dimensional square to thering is nano effect, there is again high-specific surface area and high negative charge outside surface, thereby have preferably the performances such as absorption, duct are filtered, interlayer ion exchange sterilization, physical chemistry, can be used for the processing of waste water,waste gas and industrial residue and as inorganic nano strengthening agent.
Halloysite is 1:1 dioctahedron kaolin families mineral, and structure and chemical constitution and kaolinite, dickite, nacrite are closely similar, and it is that extent of hydration is different with interlayer water content that halloysite is different from kaolinic main character.As a kind of natural clay mineral, halloysite is contained abundant, widely distributed and exploitation easier.But occurring in nature seldom has purer halloysite to occur, and is mostly to coexist with other clay mineral or impurity, as silicon-dioxide, kaolinite, illite, chlorite, gibbsite, ferric oxide etc.But because their physical and chemical performances are more approaching, general method is difficult to distinguish, thereby by people, is ignored for a long time.
Summary of the invention
The technical problem to be solved in the present invention is: for the physicochemical property of halloysite nanotubes, provide a kind of method of purification of halloysite nanotubes.The present invention adopts the dispersion suspension precipitator method to purify, and can, by the contamination precipitation in halloysite, obtain the halloysite of higher degree.
The present invention solves the technical scheme that its technical problem adopts: adopt following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 3000～5000, be dissolved in the deionized water of 380 parts, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite raw ore dispersion liquid that obtains, stir 20～30 minutes, then by 325 object filter sieve elimination impurity for mixed solution;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, standing, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified.
Inventing useful effect is: 1) due to halloysite nanotubes good dispersity in water, can form stable suspension, and its chemical property is more stable, generally be not easy to react with organic reagent, the present invention adopts the dispersion suspension precipitator method to purify, can be by contamination precipitation in halloysite, the powder (V-Brite B) that simultaneously takes a policy is removed metal oxide (as ferric oxide) as reductive agent, obtains the halloysite of higher degree.2) purification efficiency is high, can reach 70% of raw ore.3) present method is simple and quick feasible, pollution-free, can carry out industrialization production, for utilization and the research of halloysite provides the foundation.
Embodiment
Below the invention will be further described:
Embodiment 1: a kind of method of purification of halloysite nanotubes, comprises the following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 3000, be dissolved in the deionized water of 380 parts, by strong mixer, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the large beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, by strong mixer, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders (V-Brite B) as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite nanotubes raw ore dispersion liquid that obtains, by strong mixer, stir 20 minutes, then by 325 object filter sieve elimination impurity for mixed solution; The consumption of vat powder and Sodium hexametaphosphate 99 is 0.3% of liquor capacity;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, that is to say, according to adding the ratio of 4 parts of flocculant solutions to flocculate to mixed solution in the every 1000 portions of mixed solutions of mass fraction, after standing for some time, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified, the yield that obtains halloysite by quality weighing before and after purifying is about 70%.
Embodiment 2: a kind of method of purification of halloysite nanotubes, comprises the following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 5000, be dissolved in the deionized water of 380 parts, by strong mixer, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the large beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, by strong mixer, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders (V-Brite B) as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite nanotubes raw ore dispersion liquid that obtains, by strong mixer, stir 30 minutes, then by 325 object filter sieve elimination impurity for mixed solution; The consumption of vat powder and Sodium hexametaphosphate 99 is 0.3% of liquor capacity;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, that is to say, according to adding the ratio of 4 parts of flocculant solutions to flocculate to mixed solution in the every 1000 portions of mixed solutions of mass fraction, after standing for some time, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified, the yield that obtains halloysite by quality weighing before and after purifying is about 70%.
Embodiment 3: a kind of method of purification of halloysite nanotubes, comprises the following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 4000, be dissolved in the deionized water of 380 parts, by strong mixer, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the large beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, by strong mixer, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders (V-Brite B) as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite nanotubes raw ore dispersion liquid that obtains, by strong mixer, stir 25 minutes, then by 325 object filter sieve elimination impurity for mixed solution; The consumption of vat powder and Sodium hexametaphosphate 99 is 0.3% of liquor capacity;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, that is to say, according to adding the ratio of 4 parts of flocculant solutions to flocculate to mixed solution in the every 1000 portions of mixed solutions of mass fraction, after standing for some time, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified, the yield that obtains halloysite by quality weighing before and after purifying is about 70%.
Embodiment 4: a kind of method of purification of halloysite nanotubes, comprises the following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 3000, be dissolved in the deionized water of 380 parts, by strong mixer, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the large beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, by strong mixer, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders (V-Brite B) as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite nanotubes raw ore dispersion liquid that obtains, by strong mixer, stir 28 minutes, then by 325 object filter sieve elimination impurity for mixed solution; The consumption of vat powder and Sodium hexametaphosphate 99 is 0.3% of liquor capacity;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, that is to say, according to adding the ratio of 4 parts of flocculant solutions to flocculate to mixed solution in the every 1000 portions of mixed solutions of mass fraction, after standing for some time, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified, the yield that obtains halloysite by quality weighing before and after purifying is about 70%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (1)
1. a method of purification for halloysite nanotubes, is characterized in that adopting following steps:
1) by mass fraction, get 20 parts of the polyacrylamide solids of molecular weight 3000～5000, be dissolved in the deionized water of 380 parts, stir, until solid dissolves completely, obtain solid content and be 5% flocculant solution;
2) by mass fraction, get 150 parts of halloysite nanotubes raw ores, put into the beaker of 2000 milliliters, by mass fraction, add the water of 1500 parts, stir, smash halloysite raw ore, disperse, precipitate;
3) by mass fraction, get 4.5 parts of vat powders as reductive agent, 4.5 parts of Sodium hexametaphosphate 99s add step 2 as dispersion agent) in the halloysite nanotubes raw ore dispersion liquid that obtains, stir 20～30 minutes, then by 325 object filter sieve elimination impurity for mixed solution;
4) mixed solution after filtering is diluted to 3 times of volumes, in 4 parts of flocculant solutions of mass fraction, than the ratio of 1000 portions of mixed solutions, in mixed solution, add flocculant solution to flocculate, standing, elimination upper strata clear water, and with deionized water, flocculation is cleaned 2～3 times;
5) step 4) products therefrom is put in 100 ℃ of vacuum drying ovens and is dried, with mortar, grind and cross 200 object filter sieve, the halloysite nanotubes after being purified.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883390A (en) * | 2017-03-27 | 2017-06-23 | 中国地质大学（武汉） | It is a kind of to activate galapectite as the method for catalyst preparation poly epsilon caprolactone lactone |
| CN108048325A (en) * | 2017-11-28 | 2018-05-18 | 广东南芯医疗科技有限公司 | A kind of method that barium gallium manganese ion in human faecal mass is removed using lithium base galapectite |
| CN108751212A (en) * | 2018-06-14 | 2018-11-06 | 中南大学 | A kind of halloysite nanotubes material and preparation method thereof as siRNA protections |
| CN112044284A (en) * | 2019-06-06 | 2020-12-08 | 中国矿业大学(北京) | Preparation method and application of halloysite ion channel functional membrane material |
| CN112093774A (en) * | 2019-06-17 | 2020-12-18 | 中国矿业大学(北京) | Method for large-scale directional arrangement of halloysite nanotubes |
| CN113135574A (en) * | 2021-04-23 | 2021-07-20 | 中南大学 | Method for removing impurities and expanding halloysite tube cavity |
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| CN101070163A (en) * | 2007-06-12 | 2007-11-14 | 河南省科学院 | Hydrogen-store material galapectite and preparing method |
| CN101704531A (en) * | 2009-08-25 | 2010-05-12 | 中国地质大学（武汉） | Preparation method of high-purity halloysite |
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2013
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Patent Citations (2)
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| CN101070163A (en) * | 2007-06-12 | 2007-11-14 | 河南省科学院 | Hydrogen-store material galapectite and preparing method |
| CN101704531A (en) * | 2009-08-25 | 2010-05-12 | 中国地质大学（武汉） | Preparation method of high-purity halloysite |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106883390A (en) * | 2017-03-27 | 2017-06-23 | 中国地质大学（武汉） | It is a kind of to activate galapectite as the method for catalyst preparation poly epsilon caprolactone lactone |
| CN108048325A (en) * | 2017-11-28 | 2018-05-18 | 广东南芯医疗科技有限公司 | A kind of method that barium gallium manganese ion in human faecal mass is removed using lithium base galapectite |
| CN108048325B (en) * | 2017-11-28 | 2021-04-13 | 广东南芯医疗科技有限公司 | Method for removing barium, gallium and manganese ions in human excrement by using lithium-based halloysite |
| CN108751212A (en) * | 2018-06-14 | 2018-11-06 | 中南大学 | A kind of halloysite nanotubes material and preparation method thereof as siRNA protections |
| CN112044284A (en) * | 2019-06-06 | 2020-12-08 | 中国矿业大学(北京) | Preparation method and application of halloysite ion channel functional membrane material |
| CN112044284B (en) * | 2019-06-06 | 2021-07-23 | 中国矿业大学(北京) | Preparation method and application of halloysite ion channel functional membrane material |
| CN112093774A (en) * | 2019-06-17 | 2020-12-18 | 中国矿业大学(北京) | Method for large-scale directional arrangement of halloysite nanotubes |
| CN113135574A (en) * | 2021-04-23 | 2021-07-20 | 中南大学 | Method for removing impurities and expanding halloysite tube cavity |
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Application publication date: 20140226 |