CN104528750A - Method for coating whitened kaolin by sol-gel method - Google Patents
Method for coating whitened kaolin by sol-gel method Download PDFInfo
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- CN104528750A CN104528750A CN201410765759.9A CN201410765759A CN104528750A CN 104528750 A CN104528750 A CN 104528750A CN 201410765759 A CN201410765759 A CN 201410765759A CN 104528750 A CN104528750 A CN 104528750A
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Abstract
The invention discloses a method for coating whitened kaolin by a sol-gel method. The method comprises the following steps: dispersing raw kaolin ore in water to prepare kaolin pulp; adding absolute ethyl alcohol, ammonium hydroxide and tetraethyl orthosilicate to coat the surface of kaolin with tetraethyl orthosilicate hydrolyzed gel to obtain a whitened kaolin product. According to the method, iron, titanium and other coloring impurities in kaolin can be effectively blocked, so that the whiteness of a kaolin product can be remarkably improved, new impurities cannot be introduced into the kaolin raw material, and the application range of kaolin can be enlarged. The method is simple in process, low in equipment requirement, convenient to operate and low in energy consumption, can be used for producing products with stable performance, and is advantageous to large-scale popularization and application.
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 due to the kind of kaolin impurities and content thereof on product performance and range of application impact comparatively large, therefore removing impurity, to increase kaolinic whiteness is the emphasis that kaolin is studied in the industry always.
According to state and the character of impurity output, kaolin impurities can be roughly divided into following three classes: one is the organic carbon deposited together with kaolin, and its form being mixed into machinery or being wrapped in lattice exists, and makes mineral present grey black; Two is the elements such as iron, titanium with colouring power; Three is melanocratic minerals, as biotite, chlorite etc.Wherein, iron, titanium and organic carbon are the principal elements affecting kaolin whiteness, due to the content influence of iron kaolin calcined after colour generation and whiteness, thus iron contamination is topmost objectionable impurities in Production of Ceramics.Ferro element in kaolin mainly with the form existence of free iron (with independently iron mineral form) and structural iron (being present in the middle of lattice).Free iron is easily removed by physics, chemistry and biological method, and the method that prior art is commonly used has: high-temperature chlorination (calcination method), acidic treatment, flotation process, microbial oxidation, magnetic method and reduction method.But these methods cannot be removed for structural iron, also there is not yet any report about removing structural iron in kaolin at present.For this reason, if the impact that solution structural iron brings kaolin whiteness, significant role will be played to the kaolinic whiteness of raising and using value.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, there is provided that a kind of sol-gel method is coated brightens kaolinic method, by forming coating layer on kaolin particle surface, to play bridging effect to impurity such as the structural irons that can not remove, thus reach the effect significantly improving kaolin whiteness.
Object of the present invention is achieved by the following technical programs:
A kind of sol-gel method provided by the invention is coated brightens kaolinic method, comprises the following steps:
(1) kaolin raw ore and dispersion agent are added to the water, ultrasonic wave is uniformly dispersed and forms concentration is the kaolin ore slurry of 4 ~ 20wt%;
(2) described kaolin ore slurry is added absolute ethyl alcohol and stirring, then add ammoniacal liquor and tetraethoxy stirring reaction 1 ~ 3h; Wherein, the consumption of described tetraethoxy is 10 ~ 50wt% of kaolin raw ore, according to mol ratio tetraethoxy: ammoniacal liquor: ethanol=1: 2 ~ 10: 4 ~ 25; React complete after filtration, washing, dry, obtain the kaolin product brightened.
The present invention adopts tetraethoxy to be hydrolyzed in the basic conditions and forms the surface that collosol and gel is coated on kaolin particle, play bridging effect to impurity such as the structural irons in kaolin.Kaolin essential mineral is kaolinite, kaolinite is a kind of silicon aluminate crystal of stratiform, its unit cell forms kaolinite 1: 1 type sheet silicate by a tetrahedron silica sheet and an octahedra alumina sheet, along 001 aspect cleavage, usually have bottom surface (001 face) and side (010 or 110 face), kaolinite bottom surface electric charge due to its lattice cationic by the positively charged ion isomorph of low price replace and with constant negative charge; Side electric charge is that the both sexes cleavage of the oxy-compound that the siloxane bond of fracture is formed produces, positively charged in acidic medium, electronegative in alkaline medium.After adding dispersion agent, dispersant adsorption, on kaolin particle surface, improves the charge distribution on kaolin particle surface, the repulsion between particle is increased, and flucculation structure is difficult to be formed.By ammoniacal liquor adjust ph, and promote the hydrolysis of tetraethoxy, make slurries in alkaline environment, kaolinite is electronegative, and there is a large amount of hydroxyls in kaolinite particle surface, the Si-OH base condensation that kaolinite surface hydroxyl and teos hydrolysis produce is deposited on kaolinite surface and forms fine and close network packet overlay film, causes colored foreign cover screening to the iron in kaolin, thus reaches and brighten kaolinic object.
Further, in step of the present invention (1), the consumption of dispersion agent is 0.05 ~ 0.3wt% of kaolin raw ore.Described dispersion agent is Sodium hexametaphosphate 99, tripoly phosphate sodium STPP or polyaluminium sulfate.In described step (2), stirring velocity is 700 ~ 900 turns/min.
The present invention has following beneficial effect:
(1) the present invention's method of utilizing sol-gel coated, tetraethoxy is adopted to carry out coated as silicon source to kaolin, reach while brightening kaolin object, new impurity can not be introduced to kaolin starting material, can 4 ~ 6% be increased through the coated kaolin product whiteness brightened, widen kaolinic range of application, can be used as the use such as papermaking filler and ceramic raw material.
(2) present invention process is simple, and equipment requirements is low, easy to operate, and energy consumption is low, and product performance are stablized.For all significant whitening effect can not be played by the kaolin of physics, chemistry and biological method removal iron contamination or iron-removal and whitening DeGrain, be conducive to large-scale popularization and use.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail:
Fig. 1 be the coated front kaolin raw ore of example one of the present invention and through sol-gel is coated brighten after the X ray diffracting spectrum (XRD) of kaolin product;
Fig. 2 is the stereoscan photograph (SEM) of the coated front kaolin raw ore of example one of the present invention;
Fig. 3 is that example of the present invention is once the coated stereoscan photograph (SEM) brightening rear kaolin product of sol-gel.
Embodiment
Embodiment one:
The present embodiment is a kind of, and sol-gel method is coated brightens kaolinic method, and its step is as follows:
(1) add in 400mL water by 20g kaolin raw ore and 0.02g Sodium hexametaphosphate 99 dispersion agent, ultrasonic wave is dispersed into uniform kaolin ore slurry;
(2) kaolin ore slurry is added 20mL dehydrated alcohol under slow stirring, then slowly drip 8mL ammoniacal liquor and 10mL tetraethoxy, stirring reaction 1h under 700 turns/min speed; React complete after filtration, washing, dry, obtain the kaolin product brightened.
As shown in Figure 1, the kaolin raw ore before coated and coatedly brighten rear kaolin product, principal crystalline phase is kaolin and a small amount of quartz, the change that coated front and back XRD figure principal crystalline phase is too not large, mainly because coated SiO
2become amorphous state to exist, show that kaolin surface is wrapped by.
As shown in Figure 2, coated front kaolin raw ore surperficial smoother, in the form of sheets structure.
As shown in Figure 3, coated surface of brightening rear kaolin product is obviously compact, this is because progressively form silicon dioxide film at kaolin surface in the process of teos hydrolysis, condensation, surface is containing a large amount of silicone hydroxyl, and silicone hydroxyl generation polycondensation adjacent after its polymerization, forms Si-O-Si key and connect, final formation dioxide/silica gel particle film, there is small-size effect and surface-interface effect, the kaolin particle of dispersion is bonded together, illustrates that kaolin surface is wrapped by.
Embodiment two:
The present embodiment is a kind of, and sol-gel method is coated brightens kaolinic method, and its step is as follows:
(1) add in 400mL water by 30g kaolin raw ore and 0.03g tripoly phosphate sodium STPP dispersion agent, ultrasonic wave is dispersed into uniform kaolin ore slurry;
(2) kaolin ore slurry is added 30mL dehydrated alcohol under slow stirring, then slowly drip 10mL ammoniacal liquor and 12mL tetraethoxy, stirring reaction 2h under 800 turns/min speed; React complete after filtration, washing, dry, obtain the kaolin product brightened.
Embodiment three:
The present embodiment is a kind of, and sol-gel method is coated brightens kaolinic method, and its step is as follows:
(1) add in 400mL water by 40g kaolin raw ore and 0.04g polyaluminium sulfate dispersion agent, ultrasonic wave is dispersed into uniform kaolin ore slurry;
(2) kaolin ore slurry is added 40mL dehydrated alcohol under slow stirring, then slowly drip 12mL ammoniacal liquor and 14mL tetraethoxy, stirring reaction 1.5h under 900 turns/min speed; React complete after filtration, washing, dry, obtain the kaolin product brightened.
Whiteness test:
Using R457 whiteness as whiteness measuring method standard, Blue Whiteness after the calcining of the kaolin product adopting the WSD-3C type full-automatic blancometer coated front kaolin raw ore of mensuration and various embodiments of the present invention to brighten.Test result is as shown in table 1.
The test result of table 1 various embodiments of the present invention coated front and back kaolin whiteness
The present invention is a kind of, and sol-gel method is coated brightens kaolinic method, and its processing parameter is not limited to the above-mentioned embodiment enumerated.
Claims (4)
1. sol-gel method is coated brightens a kaolinic method, it is characterized in that comprising the following steps:
(1) kaolin raw ore and dispersion agent are added to the water, ultrasonic wave is uniformly dispersed and forms concentration is the kaolin ore slurry of 4 ~ 20wt%;
(2) described kaolin ore slurry is added absolute ethyl alcohol and stirring, then add ammoniacal liquor and tetraethoxy stirring reaction 1 ~ 3h; Wherein, the consumption of described tetraethoxy is 10 ~ 50wt% of kaolin raw ore, according to mol ratio tetraethoxy: ammoniacal liquor: ethanol=1: 2 ~ 10: 4 ~ 25; React complete after filtration, washing, dry, obtain the kaolin product brightened.
2. sol-gel method according to claim 1 is coated brightens kaolinic method, it is characterized in that: in described step (1), the consumption of dispersion agent is 0.05 ~ 0.3wt% of kaolin raw ore.
3. sol-gel method according to claim 1 and 2 is coated brightens kaolinic method, it is characterized in that: described dispersion agent is Sodium hexametaphosphate 99, tripoly phosphate sodium STPP or polyaluminium sulfate.
4. sol-gel method according to claim 1 is coated brightens kaolinic method, it is characterized in that: in described step (2), stirring velocity is 700 ~ 900 turns/min.
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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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| CN104528750B CN104528750B (en) | 2016-12-07 |
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Cited By (2)
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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 |
| CN114053881A (en) * | 2021-12-09 | 2022-02-18 | 天津工业大学 | Preparation method of hydrogel filtering membrane for efficiently loading catalytic organic pollutants |
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| CN101445249A (en) * | 2008-12-28 | 2009-06-03 | 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 |
| CN101774595A (en) * | 2010-01-16 | 2010-07-14 | 兖矿北海高岭土有限公司 | Process for enhanced reduction bleaching of kaolin by using thiocarbamide |
| CN102491355A (en) * | 2011-11-25 | 2012-06-13 | 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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2014
- 2014-12-12 CN CN201410765759.9A patent/CN104528750B/en not_active Expired - Fee Related
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| CN101445249A (en) * | 2008-12-28 | 2009-06-03 | 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 |
| CN101774595A (en) * | 2010-01-16 | 2010-07-14 | 兖矿北海高岭土有限公司 | Process for enhanced reduction bleaching of kaolin by using thiocarbamide |
| CN102491355A (en) * | 2011-11-25 | 2012-06-13 | 厦门大学 | Method for preparing superthin high-whiteness calcined kaolin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN114053881A (en) * | 2021-12-09 | 2022-02-18 | 天津工业大学 | Preparation method of hydrogel filtering membrane for efficiently loading catalytic organic pollutants |
| 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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