CN1248984C - High pure attapulgite clay and preparation method - Google Patents
High pure attapulgite clay and preparation method Download PDFInfo
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- CN1248984C CN1248984C CN 200410014477 CN200410014477A CN1248984C CN 1248984 C CN1248984 C CN 1248984C CN 200410014477 CN200410014477 CN 200410014477 CN 200410014477 A CN200410014477 A CN 200410014477A CN 1248984 C CN1248984 C CN 1248984C
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Abstract
The present invention discloses high purity attapulgite clay and a preparation method thereof, which belongs to the technical field of mineral resource deep processing. In the preparation method of the present invention, a physicochemical method is used for the trash extraction and the purification on natural attapulgite clay minerals to prepare the high purity attapulgite clay. The method of the present impurities is suitable for attapulgite minerals with major impurities such as dolomite or quartz sand or calcite or opal. A chemical agent is used as a purification dispersing agent to be prepared into a water solution with a certain concentration; attapulgite clay to be treated is added in the water solution at a certain temperature under the action of mechanical force; after sufficient dispersion and reaction, the attapulgite clay with perfect crystal form, white color and purity higher than 99% is obtained through separation and desiccation. The attapulgite clay can be used as additives for color ink, dyeing slurry, cosmetics, etc.
Description
Affiliated technical field
The present invention relates to a kind of high-purity attapulgite and preparation method thereof, belong to nonmetalliferous ore deep processing field.
Background technology
Attapulgite clay is called for short the silicate that recessed soil is a kind of rich magnesium, its molecular formula [Mg
5Si
8O
2o] (OH)
2(OH
2)
4.4H
2O, crystalline structure belong to 2: 1 type layer chain clay minerals, thereby give its very high use value because of its special structure and character.But because recessed soil usually and symbiosis such as rhombspar, calcite, quartz, opal, thereby directly influence its result of use and use range.
The U.S. is the state of discovery the earliest of recessed soil, also be the major country of production and the most widely used general state of research of recessed soil, purification its patent of invention U.S.Pat.No:6444601 and 6130179 about recessed Tu Kuang utilizes dispersion agent sodium polyacrylate (molecular weight 4000～5000) that recessed soil has been carried out effective dispersion purification, the domestic report that does not also have at present in this respect.
Summary of the invention
Purpose of the present invention just provides a kind of high-purity attapulgite and preparation method thereof, with the use value that improves natural attapulgite clay, expand its use range.
Technical solution of the present invention is: the clay pit that with impurity component mainly is quartz, rhombspar, lime carbonate, proteinic natural Attapulgite is after filter just, under mechanical force, its adding is mixed with in certain density sodium polyphosphate or the sodium silicate aqueous solution, at a certain temperature, be prepared into the clay ore pulp of certain density Attapulgite, after fully disperseing reaction, again through the clay or the concentrated clay ore pulp of making high-purity Attapulgite that separate, drying makes high-purity Attapulgite.It is 75-45 micron (200～325 order) that the clay pit of natural Attapulgite is just filtered fineness.Disperseing purificant is chemical pure or analytical pure, and its composition is poly-phosphate or silicate.Disperseing purificant is sodium polyphosphate or water glass.The dispersion purificant aqueous solution of preparation is homogeneous phase aqueous solution, and institute's water is a deionized water, and temperature remains on 40～80 ℃, disperse the purificant consumption according to foreign matter content in the clay pit of natural Attapulgite be handled natural Attapulgite clay pit 0.5%～3%.The clay pit add-on of natural Attapulgite is 1: 20～1: 10 with the ratio of disperseing the purificant aqueous solution.The mechanical force mode that the clay pit ore pulp of natural Attapulgite is applied is middling speed shearing force or ultra-sonic oscillation.The clay pit of natural Attapulgite fully disperses under mechanical force and under the hydration, wherein is with color substance Ti
2+With dispersion purificant generation chemical reaction, generate black TiPO
4With other impurity coprecipitation in container bottom.Adopted the mode of centrifugation or gravity settling to separate by the clay of the Attapulgite of dispersion and purifying with formed impurity.The clay of the high-purity Attapulgite after the separation makes the clay particle of required high-purity Attapulgite by air stream drying or vacuum freezedrying or spraying drying, or makes the clay slip of high-purity Attapulgite of desired concn by vacuum concentration.
Select for use inorganic salts as disperseing purificant, as silicate or poly-phosphate, not only with electrochemical action rhombspar, quartz etc. are effectively separated with the clay of Attapulgite by absorption, also can form the titanium phosphate or the titanium silicate precipitation of black simultaneously with the band colour content titanium ion in the clay of Attapulgite by chemical reaction, make the clay of Attapulgite change fish sperm look into from beige, whiteness is brought up to more than 85 from 0--40.
Purification principle of the present invention: because recessed native crystal has the good cleavage parallel with fibre axis, and layer-chain crystalline structure and fibrous fine crystals profile, Biao Mian noble potential helps aquation in addition, particularly Al
3+And Mg
2+Between extensively the having to be beneficial to and produce the active surface position and strengthen hydratability of different valency isomorphous replacement, therefore make recessed soil under impressed pressure, can fully disperse as system's shearing force or supersound process.The imbalance of surperficial inherent pore passage structure of recessed soil and surface charge forms adsorption center on recessed soil surface, therefore recessed native good adsorption performance makes and himself adsorbs big water gaging and dispersion agent and have good suspension property, thereby effectively separate with other materials such as rhombspar, quartz, calcite, opal etc., simultaneously, Ti
2++ Na
3PO
4Or NaSiO
3→ TiPO
4↓ or TiSiO
3↓+Na
+
The purify method of clay of the high-purity Attapulgite of preparation of the clay pit of natural Attapulgite is: the clay pit of the natural Attapulgite of clay content＞50% of Attapulgite just is broken to 75-45 micron (200～325 order), simultaneously with deionized water with disperse purificant to be mixed with homogeneous phase solution, wherein disperse the purificant consumption be natural Attapulgite clay pit 0.5%～3%; Under stirring state, the clay pit of the natural Attapulgite after just broken is added in the homogeneous phase solution, keeping temperature is 40～80 ℃, the clay pit add-on of natural Attapulgite is 1 with the ratio of disperseing the purificant aqueous solution: 20-1: 10, alternately shear agitation and ultra-sonic oscillation repeatedly after, separate with gravity settling equipment or separating centrifuge, remove sedimentary impurity, the clay thickness body of the Attapulgite that obtains purifying makes the clay particle of loose Attapulgite again through lyophilize or vacuum-drying or spraying drying.
Adopt the purify advantage of clay pit of natural Attapulgite of the present invention to be:
1, purifying technique is simple and easy to do, and raw material is easy to get.
2, purification back product purity height can reach 99%, and whiteness can reach more than 85.
China Soviet Union recessed native mine belt type in Anhui mainly contains recessed soil type (impurity is for a small amount of quartzy), dolomite type, opal type, montmorillonite type, and in the class of above-mentioned various ore deposits, the massfraction of the clay of Attapulgite is 10%～90%.Present method is applicable to that impurities is quartz, calcite, rhombspar, opal, and the clay pit of the natural Attapulgite of the clay content of Attapulgite＞50%.
Description of drawings
X-diffraction before and after the clay of Fig. 1 example 1 Attapulgite is purified detects figure
Scanning electron microscope detected figure before and after the clay of Fig. 2 example 1 Attapulgite was purified
X-diffraction before and after the clay of Fig. 3 example 2 Attapulgite is purified detects figure
Scanning electron microscope detected figure before and after the clay of Fig. 4 example 2 Attapulgite was purified
Embodiment
Example 1: the clay pit of the natural Attapulgite of greyish-green that contains the clay 83.8% of quartzy 17.2%, Attapulgite, just be broken to 25 microns (200 orders), by adding 40 ℃ at 1: 20, containing in the homogeneous phase aqueous solution of sodium polyphosphate 1%, after 20min mechanical stirring and 10min ultra-sonic oscillation replace each 3 times, leave standstill 30min, produce tangible canescence suspension and black precipitate layering, extract out or incline and upper strata suspension, under 80～100 ℃, carry out vacuum spray drying, the clay particle that the clay content that makes Attapulgite is 99.5%, whiteness is 87 Attapulgite.
X-diffraction, scanning electron microscope before and after the clay of Attapulgite is purified detect as depicted in figs. 1 and 2.
Example 2: the clay pit that contains the natural Attapulgite of canescence of rhombspar, quartz 47.5% just is broken to 48 microns (300 orders), contain in water glass 2.5%, 60 ℃ the homogeneous phase aqueous solution by adding at 1: 15, after 30min mechanical stirring and 20min ultra-sonic oscillation replace each 2 times, leave standstill 60min earlier, upper strata suspension is inclined to, carry out centrifugation, obtain the clay magma of Attapulgite, again through 40 ℃ of vacuum lyophilizations, the clay particle that the clay content that promptly obtains Attapulgite is 90%, whiteness is 91 Attapulgite.
X-diffraction, scanning electron microscope before and after the clay of Attapulgite is purified detect as shown in Figure 3 and Figure 4.
Claims (8)
1, the preparation method of high-purity attapulgite, it is characterized in that: the clay pit that with impurity component mainly is quartz, rhombspar, lime carbonate, proteinic natural Attapulgite is after filter just, under mechanical force, its adding is mixed with in certain density sodium polyphosphate or the sodium silicate aqueous solution, at a certain temperature, be prepared into the clay ore pulp of certain density Attapulgite, after fully disperseing reaction, again through the clay or the concentrated clay ore pulp of making high-purity Attapulgite that separate, drying makes high-purity Attapulgite.
2, the preparation method of high-purity attapulgite according to claim 1 is characterized in that: it is 75-45 micron (200～325 order) that the clay pit of natural Attapulgite is just filtered fineness.
3, the preparation method of high-purity attapulgite according to claim 1, it is characterized in that: the dispersion purificant aqueous solution of preparation is homogeneous phase aqueous solution, institute's water is a deionized water, temperature remains on 40～80 ℃, disperse the purificant consumption according to foreign matter content in the clay pit of natural Attapulgite be handled natural Attapulgite clay pit 0.5%～3%.
4, the preparation method of high-purity attapulgite according to claim 1 is characterized in that: the clay pit add-on of natural Attapulgite is 1: 20～1: 10 with the ratio of disperseing the purificant aqueous solution.
5, the preparation method of high-purity attapulgite according to claim 1 is characterized in that: the mechanical force mode that ore pulp applied of the clay pit of natural Attapulgite is middling speed shearing force or ultra-sonic oscillation.
6, the preparation method of high-purity attapulgite according to claim 1 is characterized in that: the clay of Attapulgite fully disperses under mechanical force and under the hydration, wherein is with color substance Ti
3+With dispersion purificant generation chemical reaction, generate black TiPO
4With other impurity coprecipitation in container bottom.
7, the preparation method of high-purity attapulgite according to claim 1 is characterized in that: is disperseed to separate with formed impurity with the clay employing centrifugation of the Attapulgite of purifying or the mode of gravity settling.
8, the preparation method of high-purity attapulgite according to claim 1, it is characterized in that: the clay of the high-purity Attapulgite after the separation makes the clay particle of required high-purity Attapulgite by air stream drying or vacuum freezedrying or spraying drying, or makes the clay slip of high-purity Attapulgite of desired concn by vacuum concentration.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410014477 CN1248984C (en) | 2004-03-27 | 2004-03-27 | High pure attapulgite clay and preparation method |
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|---|---|---|---|
| CN 200410014477 CN1248984C (en) | 2004-03-27 | 2004-03-27 | High pure attapulgite clay and preparation method |
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| CN1562865A CN1562865A (en) | 2005-01-12 |
| CN1248984C true CN1248984C (en) | 2006-04-05 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321934C (en) * | 2005-06-02 | 2007-06-20 | 洛阳工业高等专科学校 | Compounding for cray of playgorskite (concave-convex bar stone) and its preparation (carbonizing) process |
| CN101519209B (en) * | 2009-03-30 | 2011-05-18 | 中国科学院等离子体物理研究所 | Method for constructing attapulgite nanometer network by utilizing ion beam |
| CN101787224B (en) * | 2010-01-19 | 2013-07-17 | 江苏工业学院 | Compound of high-whiteness clay and preparation method thereof |
| CN102874826B (en) * | 2012-10-18 | 2014-05-28 | 南京信息工程大学 | Purification technical method for attapulgite clay |
| CN105271270A (en) * | 2014-07-01 | 2016-01-27 | 蒋寿悟 | High-purity attapulgite preparation method |
| CN104772107B (en) * | 2015-03-23 | 2018-03-16 | 广州优克日用品有限公司 | A kind of modified attapulgite soil material and its preparation method and application |
| CN108002400A (en) * | 2017-12-06 | 2018-05-08 | 潮州市华中陶瓷实业有限公司 | A kind of attapulgite clay product and preparation method thereof |
| CN108117266A (en) * | 2017-12-30 | 2018-06-05 | 安徽杜氏高科玻璃有限公司 | A kind of wear-resisting acid corrosion-resistant glass |
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