CN104528750B - A kind of sol-gel process cladding brightens kaolinic method - Google Patents

A kind of sol-gel process cladding brightens kaolinic method Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
kaolin
kaolinic
sol
tetraethyl orthosilicate
product
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201410765759.9A
Other languages
Chinese (zh)
Other versions
CN104528750A (en
Inventor
苏小丽
陈云霞
邹发华
曾涛
段金华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jingdezhen Ceramic Institute
Original Assignee
Jingdezhen Ceramic Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jingdezhen Ceramic Institute filed Critical Jingdezhen Ceramic Institute
Priority to CN201410765759.9A priority Critical patent/CN104528750B/en
Publication of CN104528750A publication Critical patent/CN104528750A/en
Application granted granted Critical
Publication of CN104528750B publication Critical patent/CN104528750B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

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

A kind of sol-gel process cladding brightens kaolinic method
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.
CN201410765759.9A 2014-12-12 2014-12-12 A kind of sol-gel process cladding brightens kaolinic method Expired - Fee Related CN104528750B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410765759.9A CN104528750B (en) 2014-12-12 2014-12-12 A kind of sol-gel process cladding brightens kaolinic method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410765759.9A CN104528750B (en) 2014-12-12 2014-12-12 A kind of sol-gel process cladding brightens kaolinic method

Publications (2)

Publication Number Publication Date
CN104528750A CN104528750A (en) 2015-04-22
CN104528750B true CN104528750B (en) 2016-12-07

Family

ID=52844445

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410765759.9A Expired - Fee Related CN104528750B (en) 2014-12-12 2014-12-12 A kind of sol-gel process cladding brightens kaolinic method

Country Status (1)

Country Link
CN (1) CN104528750B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

Publication number Publication date
CN104528750A (en) 2015-04-22

Similar Documents

Publication Publication Date Title
Feng et al. Dual-surface modification of calcium sulfate whisker with sodium hexametaphosphate/silica and use as new water-resistant reinforcing fillers in papermaking
CN101418140B (en) Preparation method of surface modified barium sulfate base ultrafine function powder material
US9637864B2 (en) Fibrous structured amorphous silica including precipitated calcium carbonate, compositions of matter made therewith, and methods of use thereof
CN101249965A (en) Method for preparing ultra-fine white carbon black and nano alumina by using kaolinite as raw material
CN103740139B (en) Composite titanium dioxide and preparation method thereof
CN101823722A (en) Method for preparing bentonite inorganic gel from calcium bentonite
CN101671496B (en) Method for modifying paper filler-calcium carbonate
CA2562127A1 (en) Silica-based sols and their production and use
CN102993785A (en) Preparation method for TiO2/opal composite powder material
CN106700657A (en) Surface treatment method of high-temperature-resistant nano calcium carbonate for silicone adhesives
CN104528750B (en) A kind of sol-gel process cladding brightens kaolinic method
Xue et al. Modification of wollastonite by acid treatment and alkali-induced redeposition for use as papermaking filler
CN105271344A (en) Preparation method of pine-cone-shaped calcite type micron-size calcium carbonate particles
CN109232989A (en) A kind of preparation method of rubber composite nano-calcium carbonate
Li et al. Preparation of core/shell structured silicate composite filler and its reinforcing property
CN105016343B (en) A kind of method that utilization aluminous fly-ash prepares hydrophabic silica
CN104760966B (en) A kind of method of Mechano-chemical Synthesizing lithium magnesium silicate
CN112897540A (en) Process for preparing high-whiteness composite calcium silicate by using quartz sand
Wang et al. Identifying appropriate conditions for producing spindle-like causticizing precipitated calcium carbonate for paper filler applications
CN105821703B (en) A kind of preparation method of speciality paper specific complex filler
CN104310451A (en) Preparation method of aragonite type white mud calcium carbonate
CN104004385B (en) A kind of preparation method of the modified grammite for papermaking filler
CN103466676B (en) Method for removing excess calcium oxide in white mud calcium carbonate obtained through alkali recovery
CN107417160A (en) The synthetic method of silane-modified ammonium polyacrylate water reducer under a kind of microwave action
CN103213998A (en) Purification method for improving purity of bentonite

Legal Events

Date Code Title Description
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20161207

Termination date: 20211212