CN102275946A - Method for preparing high-purity halloysite - Google Patents
Method for preparing high-purity halloysite Download PDFInfo
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- CN102275946A CN102275946A CN 201110205495 CN201110205495A CN102275946A CN 102275946 A CN102275946 A CN 102275946A CN 201110205495 CN201110205495 CN 201110205495 CN 201110205495 A CN201110205495 A CN 201110205495A CN 102275946 A CN102275946 A CN 102275946A
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Abstract
The invention relates to a method for preparing high-purity halloysite, and belongs to the field of the deep processing of minerals. The method for preparing the high-purity halloysite is characterized by comprising the following steps of: 1) preparing raw ores and water into suspension at the concentration of between 10 and 20 weight percent, wherein the halloysite accounts for 30 to 50 mass percent of raw ores; 2) adding sodium hexametaphosphate into the suspension to obtain slurry; 3) performing centrifugal separation to remove precipitates from a lower layer, taking supernatant suspension, and performing centrifugal separation again to obtain precipitates which are obtained by centrifugal separation for the second time; 4) drying the precipitates which are obtained by centrifuging for the second time at the temperature of between 80 and 100 DEG C to obtain a dried product for later use; and 5) adding concentrated hydrochloric acid into the dried product in a mass ratio of the raw ores to the hydrochloric acid of 1:30-1:70, and performing water bath and stirring at the temperature of between 70 and 80 DEG C for 1 to 10 hours; and suction-filtering the slurry obtained by stirring, washing the solid slurry until the solid slurry is neutral, and drying at the temperature of between 80 and 100 DEG C to obtain the high-purity halloysite. The purity of the halloysite prepared by the method is more than 95 percent.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity halloysite, belong to mineral deep processing field.
Technical background
(chemical ingredients is Al to halloysite
4[Si
4O
10] (OH)
84H
2O), belong to kaolinite family, claim halloysite because of its interlayer is moisture again.Under electron microscope, the halloysite external diameter of pipe is 10-50nm, and internal diameter is 5-20nm, and length is 2-40 μ m, and the crystal layer number is 15-40, has nano effect in the one dimension direction at least, and has high-specific surface area and high negative charge outside surface, is natural nano tubulose mineral.Halloysite is little except that having density, intensity is big to be waited outside the good characteristic, also have matrix is not dyeed, consistency is good, characteristics such as modified effect is obvious, being the desirable feedstock with ultra-thin fine ceramics and petroleum catalyst carrier of application value realistic, through suitably handling, is the suitable feedstock of new high-tech materials such as time release, microreactor, nanometer film assembling and surrounding purifying material with potential using value.Therefore, halloysite is the high quality raw material type that is worth very much development and use.
Halloysite is a kind of main clay mineral, is typical weathering product, and the many and clay mineral coexistence at occurring in nature is as kaolinite, illite, chlorite, gibbsite etc.Halloysite also originates in the zone of oxidation in metallic sulfide mineral deposit, also originates on a small quantity sometimes in the recent sediment, with a large amount of kaolinite symbiosis.Under the sour environment condition, normal and gibbsite and montmorillonite symbiosis.In actual applications, because their physical and chemical performances are more approaching, methods such as general using screening, flotation and hydraulic classification are difficult to distinguish, thereby halloysite often is mixed in the middle of other clay mineral, are seldom used separately.
These several years, along with the rise of mineral nano material, the special construction of halloysite also caused people's attention, and therefore, the preparation method who seeks a kind of high-purity halloysite becomes the task of top priority.
2 pieces of at present domestic research document patents about the halloysite preparation.Patent " a kind of production technique of high-purity halloysite " (CN101759195A) is passed through the kaolin slurry for preparing to cross reciprocating sieve behind the grading machine, add again afterwards and centrifugally behind the dispersion agent carry out fine gradedly, obtain high-purity halloysite (purity is greater than 90%) behind the concentrate drying; Patent " a kind of preparation method of high-purity halloysite " (CN 101704531 A) is directly halloysite raw ore slurries to be added to carry out centrifugally after dispersion agent stirs, and obtains purity after the drying greater than high-purity halloysite of 90%.
Though above-mentioned these two kinds of methods can be removed most impurity, all fail to remove gibbsite fully as the present invention.The present invention successfully removes the purity that gibbsite in the halloysite has further improved halloysite by increasing this step of pickling, reaches more than 95%, and report is not arranged at home as yet.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-purity halloysite, the purity height of the halloysite of this method preparation.
To achieve these goals, technical scheme of the present invention is: a kind of preparation method of high-purity halloysite is characterized in that it comprises the steps:
1) the quality percentage composition with halloysite is made into the suspension that concentration is 10-20wt% (quality) (containing the 10-20g raw ore in the expression 100g suspension) at raw ore and the water of 30-50%;
2) add-on by Sodium hexametaphosphate 99 is the 0.2-0.5% of ore quality, adds Sodium hexametaphosphate 99 in suspension, and mechanical stirring 2-4h obtains slurry;
3) slurry after will stirring is put into the whizzer centrifugation, rotating speed 1500-2000r/min, and the centrifugation time is 5-10min; After centrifugal, lower sediment is removed, get upper strata suspension, recentrifuge, rotating speed 3000-3800r/min, the time is 5-10min, obtains centrifugal throw out for the second time;
4) get centrifugal throw out for the second time, 80-100 ℃ of oven dry (baking 5-8h), the product after obtaining drying, standby;
5) get product after the oven dry, according to raw ore: the mass ratio of hydrochloric acid=1: 30-1: 70 ratio adds concentrated hydrochloric acid in the product after oven dry, at 70-80 ℃ of following stirring in water bath 1-10h; With the slurry suction filtration after stirring, to get solid water and be washed till neutrality, 80-100 ℃ of oven dry (baking 2-4h) obtains high-purity halloysite (product).
Described raw ore comprises natural halloysite, and the main composition of natural halloysite comprises halloysite, kaolinite, illite, gibbsite, quartz and feldspar.
Principle of the present invention is: utilize the special hydrating capacity of halloysite, can obtain extremely strong dispersion suspension in water, then by high speed centrifugation, remove the kaolin, illite and other heavy mineral that contain in the raw ore; Remaining gibbsite is dissolved (this method can be removed gibbsite fully) by adding acid, thereby obtain highly purified halloysite product, the purity of halloysite is greater than 95% (quality).Technology of the present invention is simple, and is easy to operate, and preparation cost is low, the purification efficiency height, and especially Zhi Bei halloysite purity is very high.
Description of drawings
Fig. 1 is the XRD figure spectrum of raw ore.
Fig. 2 is the XRD figure spectrum of the embodiment of the invention 1 resulting product.
Fig. 3 is the XRD figure spectrum of the embodiment of the invention 2 resulting products.
Fig. 4 is the XRD figure spectrum of the embodiment of the invention 3 resulting products.
Fig. 5 is the field emission scanning electron microscope photo of the embodiment of the invention 1 resulting product.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with example, but the present invention not only is confined to the following examples.
Embodiment 1:
A kind of preparation method of high-purity halloysite, it comprises the steps:
1) be that 50% natural halloysite raw ore (the main composition of natural halloysite comprises halloysite, kaolinite, illite, gibbsite, quartz and feldspar, sees Fig. 1) and water are made into the suspension that concentration is 20wt% (quality) (containing the 20g raw ore in the expression 100g suspension) with the quality percentage composition of halloysite;
2) add-on by Sodium hexametaphosphate 99 is 0.2% of an ore quality, adds Sodium hexametaphosphate 99 in suspension, and mechanical stirring 3h obtains slurry;
3) slurry after will stirring is put into the whizzer centrifugation, rotating speed 2000r/min, and the time is 10min; After centrifugal, lower sediment is removed, get upper strata suspension, recentrifuge, rotating speed 3800r/min, time 10min obtains centrifugal throw out for the second time;
4) get centrifugal throw out for the second time, 100 ℃ of oven dry (baking 5h), the product after obtaining drying, standby;
5) get product after the oven dry, according to natural halloysite raw ore: the ratio of the mass ratio of hydrochloric acid=1: 50 adds concentrated hydrochloric acid (concentration of concentrated hydrochloric acid is 36-38%), at 70 ℃ of following stirring in water bath 10h in the product after the oven dry; With the slurry suction filtration after stirring, to get solid water and be washed till neutrality, 100 ℃ of oven dry (baking 2h) obtain high-purity halloysite (product).
The XRD figure spectrum of high-purity halloysite (product) as can be seen, is not almost seen other impurity peaks as shown in Figure 2 in the collection of illustrative plates, the purity of halloysite product is greater than 96% (quality).The field emission scanning electron microscope photo of product as shown in Figure 5, visible significantly multilayer hollow tubular structures is typical halloysite microscopic appearance feature among the figure.
Embodiment 2:
A kind of preparation method of high-purity halloysite, it comprises the steps:
1) be that 40% natural halloysite raw ore (the main composition of natural halloysite comprises halloysite, kaolinite, illite, gibbsite, quartz and feldspar, sees Fig. 1) and water are made into the suspension that concentration is 15wt% (quality) (containing the 15g raw ore in the expression 100g suspension) with the quality percentage composition of halloysite;
2) add-on by Sodium hexametaphosphate 99 is 0.3% of an ore quality, adds Sodium hexametaphosphate 99 in suspension, and mechanical stirring 2h obtains slurry;
3) slurry after will stirring is put into the whizzer centrifugation, rotating speed 2000r/min, time 5min; After centrifugal, lower sediment is removed, get upper strata suspension, recentrifuge, rotating speed 3000r/min, time 5min obtains centrifugal throw out for the second time;
4) get centrifugal throw out for the second time, 100 ℃ of oven dry (5h), the product after obtaining drying, standby;
5) get product after the oven dry, according to natural halloysite raw ore: the ratio of the mass ratio of hydrochloric acid=1: 30 adds concentrated hydrochloric acid in the product after oven dry, at 80 ℃ of following stirring in water bath 5h; With the slurry suction filtration after stirring, to get solid water and be washed till neutrality, 100 ℃ of oven dry (baking 2h) obtain high-purity halloysite (product).
The XRD figure spectrum of high-purity halloysite (product) as can be seen, is not almost seen other impurity peaks as shown in Figure 3 in the collection of illustrative plates, the purity of halloysite product is greater than 98% (quality).From the field emission scanning electron microscope photo of product, visible significantly multilayer hollow tubular structures is typical halloysite microscopic appearance feature.
Embodiment 3:
A kind of preparation method of high-purity halloysite, it comprises the steps:
1) be that the natural halloysite raw ore (the main composition of natural halloysite comprises halloysite, kaolinite, illite, gibbsite, quartz and feldspar, sees Fig. 1) and the water of 30% (quality) is made into the suspension that concentration is 10% (quality) (containing the 10g raw ore in the expression 100g suspension) with the quality percentage composition of halloysite;
2) add-on by Sodium hexametaphosphate 99 is 0.5% of an ore quality, adds Sodium hexametaphosphate 99 in suspension, and mechanical stirring 4h obtains slurry;
3) slurry after will stirring is put into the whizzer centrifugation, rotating speed 1500r/min, time 10min; After centrifugal, lower sediment is removed, get upper strata suspension, recentrifuge, rotating speed 3800r/min, time 5min obtains centrifugal throw out for the second time;
4) get centrifugal throw out for the second time, 80 ℃ of oven dry (baking 8h), the product after obtaining drying, standby;
5) get product after the oven dry, according to natural halloysite raw ore: the ratio of the mass ratio of hydrochloric acid=1: 70 adds concentrated hydrochloric acid in the product after oven dry, at 70 ℃ of following stirring in water bath 1h; With the slurry suction filtration after stirring, to get solid water and be washed till neutrality, 80 ℃ of oven dry (baking 4h) obtain high-purity halloysite (product).
The XRD figure spectrum of product as can be seen, is not almost seen other impurity peaks as shown in Figure 4 in the collection of illustrative plates, the purity of halloysite product is greater than 95% (quality).From the field emission scanning electron microscope photo of product, visible significantly multilayer hollow tubular structures is typical halloysite microscopic appearance feature.
Claims (2)
1. the preparation method of a high-purity halloysite is characterized in that it comprises the steps:
1) the quality percentage composition with halloysite is made into the suspension that concentration is 10-20wt% at raw ore and the water of 30-50%;
2) add-on by Sodium hexametaphosphate 99 is the 0.2-0.5% of ore quality, adds Sodium hexametaphosphate 99 in suspension, and mechanical stirring 2-4h obtains slurry;
3) slurry after will stirring is put into the whizzer centrifugation, rotating speed 1500-2000r/min, and the centrifugation time is 5-10min; After centrifugal, lower sediment is removed, get upper strata suspension, recentrifuge, rotating speed 3000-3800r/min, the time is 5-10min, obtains centrifugal throw out for the second time;
4) get centrifugal throw out for the second time, 80-100 ℃ of oven dry, the product after obtaining drying, standby;
5) get product after the oven dry, according to raw ore: the mass ratio of hydrochloric acid=1: 30-1: 70 ratio adds concentrated hydrochloric acid in the product after oven dry, at 70-80 ℃ of following stirring in water bath 1-10h; With the slurry suction filtration after stirring, to get solid water and be washed till neutrality, 80-100 ℃ of oven dry obtains high-purity halloysite.
2. the preparation method of a kind of high-purity halloysite according to claim 1, it is characterized in that: described raw ore comprises natural halloysite.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102658099A (en) * | 2012-04-20 | 2012-09-12 | 浙江理工大学 | Method for preparing humidity-controlling material with nanotube structure |
| CN102992348A (en) * | 2012-12-10 | 2013-03-27 | 中国地质大学（武汉） | Method for preparing Al-SBA-15 ordered mesoporous composite material by taking halloysite as raw material |
| CN104497988A (en) * | 2015-01-12 | 2015-04-08 | 兰州理工大学 | Kaolin phase-change composite energy storage material and preparation method thereof |
| CN106212450A (en) * | 2016-07-21 | 2016-12-14 | 河南师范大学 | A kind of modified halloysite nanotubes composite sustained-release pesticides and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704531A (en) * | 2009-08-25 | 2010-05-12 | 中国地质大学（武汉） | Preparation method of high-purity halloysite |
| CN102091609A (en) * | 2010-12-03 | 2011-06-15 | 于向真 | Modified clay new material and preparation method thereof |
-
2011
- 2011-07-21 CN CN 201110205495 patent/CN102275946A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704531A (en) * | 2009-08-25 | 2010-05-12 | 中国地质大学（武汉） | Preparation method of high-purity halloysite |
| CN102091609A (en) * | 2010-12-03 | 2011-06-15 | 于向真 | Modified clay new material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102658099A (en) * | 2012-04-20 | 2012-09-12 | 浙江理工大学 | Method for preparing humidity-controlling material with nanotube structure |
| CN102992348A (en) * | 2012-12-10 | 2013-03-27 | 中国地质大学（武汉） | Method for preparing Al-SBA-15 ordered mesoporous composite material by taking halloysite as raw material |
| CN102992348B (en) * | 2012-12-10 | 2014-04-09 | 中国地质大学（武汉） | Method for preparing Al-SBA-15 ordered mesoporous composite material by taking halloysite as raw material |
| CN104497988A (en) * | 2015-01-12 | 2015-04-08 | 兰州理工大学 | Kaolin phase-change composite energy storage material and preparation method thereof |
| CN106212450A (en) * | 2016-07-21 | 2016-12-14 | 河南师范大学 | A kind of modified halloysite nanotubes composite sustained-release pesticides and preparation method thereof |
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Application publication date: 20111214 |