CN104528750B - A kind of sol-gel process cladding brightens kaolinic method - Google Patents
A kind of sol-gel process cladding brightens kaolinic method Download PDFInfo
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- CN104528750B CN104528750B CN201410765759.9A CN201410765759A CN104528750B CN 104528750 B CN104528750 B CN 104528750B CN 201410765759 A CN201410765759 A CN 201410765759A CN 104528750 B CN104528750 B CN 104528750B
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- kaolin
- kaolinic
- sol
- tetraethyl orthosilicate
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Abstract
The invention discloses a kind of sol-gal process cladding and brighten kaolinic method, kaolin raw ore is dispersed in water and is configured to kaolin ore slurry, it is subsequently adding dehydrated alcohol, ammonia and tetraethyl orthosilicate so that teos hydrolysis gelling is coated on kaolinic surface and obtains the kaolin product brightened.The coloring impurity such as the ferrotitanium in Kaolin can be played and effectively cover effect by the present invention, thus significantly improve the whiteness of kaolin product, and kaolin starting material will not be introduced new impurity, widened kaolinic range of application.Present invention process is simple, and equipment requirements is low, easy to operate, and energy consumption is low, and properties of product are stable, is conducive to large-scale popularization and use.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, particularly relate to a kind of method increasing Kaolin whiteness.
Background technology
Kaolin, as a kind of important inorganic non-metallic raw material, is widely used in the industries such as coating, papermaking and pottery.But
Owing to properties of product and range of application are affected relatively big by kind and the content thereof of Kaolin impurities, the removal of impurity is therefore gone to increase
Add kaolinic whiteness and be always the emphasis that Kaolin is studied in the industry.
According to state and the character of impurity output, Kaolin impurities can be roughly divided into following three classes: one is and kaolinite
The organic carbon that soil deposits together, presented in it is mixed into by machinery or is wrapped in lattice so that mineral present grey black；
Two is to have the elements such as the ferrum of colouring power, titanium；Three is melanocratic mineral, such as biotite, chlorite etc..Wherein, ferrum, titanium and organic
Carbon is the principal element affecting Kaolin whiteness, due to the content of ferrum affect kaolin calcined after in normal complexion whiteness, thus ferrum
Impurity is topmost harmful substance in Production of Ceramics.Ferrum element in Kaolin main with free ferrum (with independent iron mineral
Form) and structural iron (being present in the middle of lattice) presented in.Free ferrum goes easily by physics, chemical and biological method
Removing, the method that prior art is commonly used has: high-temperature chlorination (calcination method), acidic treatment, floatation, microbial oxidation, magnetic separation
Method and reducing process.But these methods cannot be removed for structural iron, currently also there is not yet about removing structure in Kaolin
Any report of ferrum.To this end, if solving the impact that Kaolin whiteness is brought by structural iron, will be to improving kaolinic whiteness
Significant role is played with using value.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of sol-gel process cladding brightens Kaolin
Method, by kaolin particle surface formed clad, so that the impurity such as the structural iron that can not remove are played bridging effect,
Thus reach to significantly improve the effect of Kaolin whiteness.
The purpose of the present invention is achieved by the following technical programs:
A kind of sol-gel process cladding that the present invention provides brightens kaolinic method, comprises the following steps:
(1) kaolin raw ore and dispersant being added to the water, ultrasound wave is uniformly dispersed and forms the height that concentration is 4～20wt%
Ridge soil ore pulp；
(2) described kaolin ore slurry is added absolute ethyl alcohol and stirring, be subsequently adding ammonia and tetraethyl orthosilicate stirring reaction 1
～3h；Wherein, the consumption of described tetraethyl orthosilicate is the 10～50wt% of kaolin raw ore, according to mol ratio tetraethyl orthosilicate:
Ammonia: ethanol=1: 2～10: 4～25；React complete through filtering, washing, be dried, obtain the kaolin product brightened.
The present invention uses tetraethyl orthosilicate to hydrolyze to form collosol and gel in the basic conditions and is coated on the table of kaolin particle
Face, plays bridging effect to impurity such as the structural irons in Kaolin.Kaolin essential mineral is kaolinite, and kaolinite is a kind of layer
The silicon aluminate crystal of shape, its unit cell is formed kaolinite 1: 1 by a tetrahedron silica sheet and an octahedra alumina sheet
Type sheet silicate, along 001 aspect cleavage, generally has bottom surface (001 face) and side (010 or 110 face), kaolinite bottom surface electric charge
Due to its lattice cationic by the cation isomorph replacement of low price with constant negative charge；Side electric charge is fracture
The both sexes cleavage of hydroxy compounds that formed of siliconoxygen bond and produce, positively charged in acid medium, in alkaline medium, band is negative
Electric charge.After adding dispersant, dispersant adsorption is on kaolin particle surface, and the electric charge improving kaolin particle surface divides
Cloth, makes the repulsion between granule increase, and flocculent structure is difficult to be formed.Regulate pH value by ammonia, and promote tetraethyl orthosilicate
Hydrolysis, makes serosity in alkaline environment, and kaolinite is electronegative, and kaolinite particle surface exists substantial amounts of hydroxyl, kaolinite
The Si-OH base condensation that surface hydroxyl and teos hydrolysis produce is deposited on kaolinite surface and forms the network cladding of densification
Film, covers screening to the ferrum coloring impurity in Kaolin, thus reaches to brighten kaolinic purpose.
Further, in step of the present invention (1) consumption is kaolin raw ore the 0.05～0.3wt% of dispersant.
Described dispersant is sodium hexameta phosphate, sodium tripolyphosphate or polyaluminium sulfate.In described step (2), mixing speed is 700～900
Turn/min.
The method have the advantages that
(1) present invention utilizes the method that sol-gel is coated with, and uses tetraethyl orthosilicate to wrap Kaolin as silicon source
Cover, while reaching to brighten Kaolin purpose, kaolin starting material will not be introduced new impurity, through the Kaolin that cladding brightens
Product whiteness can increase by 4～6%, has widened kaolinic range of application, can use as papermaking filler and Ceramic Material etc..
(2) present invention process is simple, and equipment requirements is low, easy to operate, and energy consumption is low, and properties of product are stable.For not leading to
Crossing physics, chemistry and biological method goes the Kaolin of iron impurity or iron-removal and whitening DeGrain all can play significantly increasing
White effect, is conducive to large-scale popularization and uses.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail:
Fig. 1 be present example one be coated with front kaolin raw ore and after sol-gel cladding brightens the X of kaolin product
X ray diffraction collection of illustrative plates (XRD)；
Fig. 2 is the stereoscan photograph (SEM) that present example one is coated with front kaolin raw ore；
Fig. 3 is that present example brightens the stereoscan photograph (SEM) of rear kaolin product once sol-gel cladding.
Detailed description of the invention
Embodiment one:
The present embodiment one sol-gel process cladding brightens kaolinic method, and its step is as follows:
(1) 20g kaolin raw ore and 0.02g sodium hexameta phosphate dispersant being added in 400mL water, ultrasound wave is dispersed into all
Even kaolin ore slurry；
(2) kaolin ore slurry is added under slow stirring 20mL dehydrated alcohol, be then slowly added dropwise 8mL ammonia and 10mL
Tetraethyl orthosilicate, stirring reaction 1h under 700 turns/min speed；React complete through filtering, washing, be dried, obtain the height brightened
Ridge native produce.
As it is shown in figure 1, kaolin raw ore and cladding before Bao Fu brighten rear kaolin product, principal crystalline phase be Kaolin and
A small amount of quartz, before and after cladding, XRD figure principal crystalline phase does not has the biggest change, is primarily due to the SiO of cladding2Become amorphous state
Exist, show that kaolin surface is wrapped by.
As in figure 2 it is shown, the kaolin raw ore surface smoother before Bao Fu, structure in the form of sheets.
As it is shown on figure 3, the surface that cladding brightens rear kaolin product is the compactest, this is because at tetraethyl orthosilicate water
Progressively forming silicon dioxide film at kaolin surface during solution, condensation, substantial amounts of silicone hydroxyl is contained on surface, phase after its polymerization
Adjacent silicone hydroxyl generation polycondensation reaction, forms Si-O-Si bonded, ultimately forms dioxide/silica gel particle film, have small size
Effect and surface-interface effect, be bonded together scattered Kaolin particle, illustrate that kaolin surface is wrapped by.
Embodiment two:
The present embodiment one sol-gel process cladding brightens kaolinic method, and its step is as follows:
(1) 30g kaolin raw ore and 0.03g sodium tripolyphosphate dispersant being added in 400mL water, ultrasound wave is dispersed into all
Even kaolin ore slurry；
(2) kaolin ore slurry is added under slow stirring 30mL dehydrated alcohol, be then slowly added dropwise 10mL ammonia and
12mL tetraethyl orthosilicate, stirring reaction 2h under 800 turns/min speed；React complete through filtering, washing, be dried, brightened
Kaolin product.
Embodiment three:
The present embodiment one sol-gel process cladding brightens kaolinic method, and its step is as follows:
(1) 40g kaolin raw ore and 0.04g polyaluminium sulfate dispersant being added in 400mL water, ultrasound wave is dispersed into all
Even kaolin ore slurry；
(2) kaolin ore slurry is added under slow stirring 40mL dehydrated alcohol, be then slowly added dropwise 12mL ammonia and
14mL tetraethyl orthosilicate, stirring reaction 1.5h under 900 turns/min speed；React complete through filtering, washing, be dried, increased
White kaolin product.
Whiteness test:
Using R457 whiteness as whiteness measuring method standard, the full-automatic leucometer of WSD-3C type is used to measure kaolinite before cladding
Blue Whiteness after the calcining of the kaolin product that soil raw ore and various embodiments of the present invention brighten.Test result is as shown in table 1.
The test result of Kaolin whiteness before and after table 1 various embodiments of the present invention cladding
One sol-gel process of the present invention cladding brightens kaolinic method, and its technological parameter is not limited to above-mentioned enumerating
Embodiment.
Claims (1)
1. a sol-gel process cladding brightens kaolinic method, it is characterised in that comprise the following steps:
(1) kaolin raw ore and dispersant being added to the water, ultrasound wave is uniformly dispersed and forms the Kaolin that concentration is 4～20wt%
Ore pulp；Described dispersant is sodium hexameta phosphate, sodium tripolyphosphate or polyaluminium sulfate, its consumption be kaolin raw ore 0.05～
0.3wt%；
(2) described kaolin ore slurry is added absolute ethyl alcohol and stirring, be subsequently adding ammonia and tetraethyl orthosilicate low whipping speed 700
～stirring reaction 1～3h under 900 turns/min；Wherein, the consumption of described tetraethyl orthosilicate is the 10～50wt% of kaolin raw ore,
According to mol ratio tetraethyl orthosilicate: ammonia: ethanol=1: 2～10: 4～25；React complete through filtering, washing, be dried, increased
White kaolin product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410765759.9A CN104528750B (en) | 2014-12-12 | 2014-12-12 | A kind of sol-gel process cladding brightens kaolinic method |
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| CN201410765759.9A CN104528750B (en) | 2014-12-12 | 2014-12-12 | A kind of sol-gel process cladding brightens kaolinic method |
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| CN104528750A CN104528750A (en) | 2015-04-22 |
| CN104528750B true CN104528750B (en) | 2016-12-07 |
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| CN111410204A (en) * | 2020-05-08 | 2020-07-14 | 鑫中科贸易(深圳)有限公司 | Method for preparing high-grade kaolin from sludge soil |
| CN114053881B (en) * | 2021-12-09 | 2024-04-05 | 上海源依青科技有限责任公司 | Preparation method of hydrogel filtering membrane for efficiently loading and catalyzing organic pollutants |
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| CN101445249B (en) * | 2008-12-28 | 2010-09-01 | 梁明 | Method for bleaching high-concentration kaolin pulp |
| CN101671033A (en) * | 2009-09-27 | 2010-03-17 | 福建师范大学 | Biological iron-removal and whitening method for kaolin by iron reduction bacillus taking molasses as carbon sources |
| CN101774595B (en) * | 2010-01-16 | 2011-11-09 | 兖矿北海高岭土有限公司 | Process for enhanced reduction and bleaching of kaolin by using thiocarbamide |
| CN102491355B (en) * | 2011-11-25 | 2013-09-18 | 厦门大学 | Method for preparing superthin high-whiteness calcined kaolin |
| CN103193241A (en) * | 2013-03-20 | 2013-07-10 | 中国地质大学（武汉） | Method for improving whiteness of metakaolin through utilizing natural biomass raw material |
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Granted publication date: 20161207 Termination date: 20211212 |