CN108727874A - A kind of preparation method of silicon titanium composite granule - Google Patents
A kind of preparation method of silicon titanium composite granule Download PDFInfo
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- CN108727874A CN108727874A CN201810603701.2A CN201810603701A CN108727874A CN 108727874 A CN108727874 A CN 108727874A CN 201810603701 A CN201810603701 A CN 201810603701A CN 108727874 A CN108727874 A CN 108727874A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
Abstract
A kind of preparation method of silicon titanium composite granule, belongs to composite granule technical field.The present invention makes silicon titanium particle stroke deposition cladding by wet method organic surface modifying, eventually passes through roasting increase titanyl silicon key and is formed, reduce the quantity of hydrogen bond, increases stability, improves the table specific area of titanium to increase coloration.
Description
Technical field
The invention belongs to composite granule technical fields, and in particular to titanium dioxide and silicon powder, the silicon titanium composite granule have
Good dispersibility is with stability and optical property suitable with titanium dioxide.
Background technology
Titanium dioxide is the white inorganic pigment that performance is best so far, be widely used in coating, plastics, ink, papermaking,
The fields such as rubber, chemical fibre and cosmetics.But substantially high situation allows one for its expensive price and in this year price
A little downstream users are suffered untold misery, titanium dioxide price continuous rise since 2016, since 2016, have been looked up with whole,
Titanium dioxide price continuous rise.On May 8th, 2017, Huntsman announce to raise the price in the world about 250 beautiful yuan/ton again；
Domestic 15 collectives of titanium dioxide enterprise publication appreciated and notified on October 12nd, 2017, and up-regulation price range is 500 yuan/ton.At present
Domestic East China rutile-type product market price is 19800 yuan/ton, compares 10500 yuan/ton at the beginning of 2016 of low spot amount of increase
By about one time.From the beginning of this year, it is influenced by environmental protection regulation, domestic ilmenite concentrate price persistently rises, and Sichuan climbs steel recent quotation and is
1950 yuan/ton, compared to 2016 at the beginning of 630 yuan/ton of low spot amount of increase surpassed 200%.
Therefore many researchers and enterprise are dedicated to developmental research mineral/titanium dioxide composite particulate material, to prepare
High-performance, the titanium dioxide substitute of low price.The silicon titanium composite granule price cheap with respect to titanium dioxide about one of my team's research and development
Half, suppleness and titanium dioxide are suitable；The pigment performance of titanium dioxide is embodied by optical property, and optical property depends primarily on two
The surface nature of Titanium particles, kernel hardly play a role, my the silicon titanium composite granule titanium dioxide of team's research is accurate
It is intact that coated silica makes surface remain titanium dioxide optics performance；And titanium dioxide plays contribution face with 20% ratio
Material covers 80% or more contribution, simultaneously because the addition of silica improves the dispersibility of titanium dioxide.
By preparing mineral-TiO similar with titanium dioxide performance2Composite pigment is alleviated in titanium white production and application
The effective measures of the problems such as existing resource, environment and cost price, while also helping the efficient utilization of mineral resources.This group
The active micro silicon powder and titanium dioxide that team develops produce composite pigment, and the production key of active micro silicon powder is silica surface
Modified technique, surface, which is modified, is divided into chemical modification processing and heat treatment two procedures.By chemical surface modification treated grain
Son needs further heat treatment drying.Silica surface hygroscopic capacity is low after heat treatment, and filled articles hygroscopic capacity also significantly under
Drop.But only by heat treatment, the bonding effect at interface when cannot improve filling very well, so before heat treatment, often to thin
Particle silica is using zinc compound or using silane (silane coupling agent) and transition metal ions to fine particle titanium dioxide
Silicon is handled.Key issues of scale around silicon powder surface and interface hydrophilic-lipophilic balance (HLB) is modified, team develops surface
Modified new strategy, has opened up surface modification-dried in place deshydroxy process route, has succeeded in developing with high lipophilic comprehensive silicon
The large-scale production proprietary technology of micro mist series of products.
Secondly the active micro silicon powder used in us mainly uses good natural silicon ore, different in nucleus by detaching
The complex technologies such as class mineral element and disintegration hydroxyl, realization both solve to improve purity problem, while the secondary dirt in process flow
Chronic disease is contaminated, the purpose of pure keeping purification, natural silicon ore (SiO are reached2) through exploiting, being crushed, sand processed, magnetic separation, flotation, roasting, acid
It washes, purify, the multiple tracks technique such as high-purity water process is processed into silicon powder.
Invention content
The object of the present invention is to provide a kind of preparation methods of silicon titanium composite granule so that silicon titanium composite granule has good
Dispersibility with stability and optical property suitable with titanium dioxide.
To achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of silicon titanium composite granule, which is characterized in that including effective procedure：
Step 1：Prepare the dispersion liquid of active micro silicon powder
By surface contain great amount of hydroxy group and form hydrophilic silicon powder i.e. active micro silicon powder and be scattered in absolute ethyl alcohol,
It is preferred that corresponding to 5-15L absolute ethyl alcohols per 5kg active micro silicon powders.
The present invention solves disadvantage of the silicon powder in organic resin application using active micro silicon powder, not only increases and has
The compatibility of machine resin effectively reduces cost also so that loading greatly increases.Therefore, active micro silicon powder is in coating industry
Application can be described as " having boundless prospects ".Active micro silicon powder surface is hydrophilic, and no matter vapor phase method or the precipitation method are not always the case.
The great amount of hydroxy group that active micro silicon powder surface is rich in, can improve particle and intermolecular compatibility, reinforcing filler and polymer it
Between reciprocation, improve process industrial art performance, improve the reinforcing property of filler.
What active micro silicon powder used in the present invention can be prepared or was commercialized, such as purchase limited public affairs of Son new material in Nanjing
Department.
Step 2：The preparation of nanoscale titanium hydroxide colloidal sol
Under stirring conditions by butyl titanate, to the continuous spray water in its surface and the mixed solution for slowing down agent, make metatitanic acid
Butyl ester complete hydrolysis, therein to slow down agent be that can slow down the reagent of butyl titanate hydrolysis rate, water and slows down the ratio of agent not
Limit, a small amount of mixed solution can be sprayed repeatedly, every time less by slowing down agent content, and slowing down agent content mostly can largely spray mixed solution.
The titania sources compound hydrolysis such as present invention butyl titanate prepare Nano titanium dioxide, due to butyl titanate height
Activity can provide Quick cross-linking reaction, improve the performance of Polyester Paint if the reactive group activity of adhesive resin is relatively low when use
With as preparing high-temperature resistant coating.While cross-linking reaction, butyl titanate can improve the adhesiveness of polymer, improve ink pair
The adhesive force of system.
Butyl titanate is the common raw material that sol-gal process prepares nano-titanium dioxide, because its hydrolysis is too violent, therefore is often added
Ethyl alcohol, glacial acetic acid, diethanol amine etc. it is miscible with water slow down hydrolysis rate.
Butyl titanate hydrolyzes with water in medium ethyl alcohol and generates Ti (OH)4, it is main that butyl titanate hydrolyzes in ethanol medium
Step, reaction is wanted to be made of the following steps；
Ti(O-Bu)4+H2O→Ti(O·Bu)3(OH)+C4H9OH
Ti(O-Bu)3(OH)+H2O→Ti(O-Bu)2(OH)2+C4H9OH
Ti(O-Bu)2(OH)2+H2O→Ti(O-Bu)(OH)3+C4H9OH
Ti(O-Bu)(OH)3+H2O→Ti(OH)4+C4H9OH
Net reaction is as follows:
Ti(O-Bu)4+4H2O→Ti(OH)4+4C4H9OH
Step 3：Final silicon titanium is compound
Nano level dioxy prepared by the dispersion liquid and step 2 of the active micro silicon powder finally prepared by above-mentioned steps one
It is compound to change titanium progress, two kinds of samples are put into high speed agitator and are mixed, carrying out at least one hour high-speed stirred keeps its compound
It is even, incubation is deposited later one hour, the titanium hydroxide colloidal sol that the titania sources compound such as butyl titanate is formed after hydrolyzing
Active micro silicon powder particle surface is coated, after depositing incubation, centrifugal solid-liquid separation is carried out, passes through 800 DEG C -900 DEG C later
Roasting is high temperature inert atmosphere heat treatment dehydration structure silica titanium key, the titanium dioxide crystal form being formed simultaneously in high temperature inert gas
It is converted to rutile-type, forms the silicon dioxide composite powder of rutile titanium dioxide cladding.
The present invention makes silicon titanium particle stroke deposition cladding by wet method organic surface modifying, eventually passes through roasting and increases titanyl
Silicon key is formed, and the quantity of hydrogen bond is reduced, and is increased stability, is improved the table specific area of titanium to increase coloration.
Different silicon titanium molar ratios can be adjusted when preparing silicon titanium composite granule, general silicon titanium than the smaller the better, in conjunction with into
Row and the synthesis of effect are preferred (1-4):1.
For example silicon titanium is prepared than difference, need the raw material for matching different amounts, correspondence to meet no industry demand.
The advantage of the invention is that：
1. by it is compound we the optical property of titanium has been fully retained, only with 20% titanium surface recombination i.e. reach titanium white
The coloration of powder.
2. reducing the formation of hydrogen bond after high-temperature calcination, the formation of silica titanium key is increased, the steady of composite granule is increased
It is qualitative.And titanium dioxide crystal form is converted to rutile-type, compares anatase and is easier to be uniformly dispersed, is formed by composite powder
Body is more uniform, it is made to be more applicable for the industries such as various building coatings, industrial paint, anti-decaying paint, ink, powdery paints.
3. the needs in order to meet different businessmans can flexibly allocate silicon titanium ratio
4. the cost of material used in the present invention is cheap relative to titanium dioxide, silicon titanium ratio is 4：Cost is taken around when 1
0.81 ten thousand yuan.
Description of the drawings
Fig. 1 is the preparation flow figure of silicon titanium composite granule of the present invention；
Fig. 2 is the formation schematic diagram of silicon titanium recombination reaction structure chart-silica titanium key；
Fig. 3 is silicon titanium recombination reaction structure chart --- the formation schematic diagram of hydrogen bond；
Fig. 4 is silicon titanium molar ratio 2:The SEM of 1 silicon titanium composite granule schemes
Fig. 5 silicon titaniums molar ratio 2:1 sample EDX analysis data (Al, C element of the inside etc. are probably derived from silicon powder)
Fig. 6 silicon titaniums molar ratio 2:The XRD diagram of titanium dioxide in 1 sample；
Specific implementation mode
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
(1) dispersion liquid of active micro silicon powder is prepared
5kg active micro silicon powders are dispersed in the dispersion liquid that active micro silicon powder is formed in 10L absolute ethyl alcohols；Activated silica is micro-
Powder is bought in Nanjing ZhongSun new materials Co., Ltd.
(2) preparation of nanoscale titanium hydroxide colloidal sol
Under stirring conditions by butyl titanate, to its surface spray water and mixed solution (the metatitanic acid fourth for slowing down agent ethyl alcohol
The volume ratio 2 of ester, water, ethyl alcohol:1:2), make butyl titanate complete hydrolysis.
(3) finally the dispersion liquid of the active micro silicon powder of above-mentioned preparation and the nano level titanium dioxide of preparation are answered
It closes, two kinds of samples is put into high speed agitator and are mixed, carrying out at least one hour high-speed stirred keeps its compound uniformly, deposits later
Incubation one hour, the titanium hydroxide Sol-gel Coated activated silica that the titania sources compound such as butyl titanate is formed after hydrolyzing are micro-
Powder particles surface, after depositing incubation, carries out centrifugal solid-liquid separation, passes through in 850 DEG C of high temperature inert gas roasting later
I.e. high temperature inert atmosphere heat treatment dehydration structure silica titanium key, the titanium dioxide crystal form being formed simultaneously are converted to rutile-type, shape
The silicon dioxide composite powder coated at rutile titanium dioxide.
Following difference aberration report form corresponds to data of the different silicon titaniums than experiment respectively.
Aberration reports (one)
Aberration reports (two)
Aberration reports (three)
Aberration reports (four)
The test of various aspects is carried out to composite granule, it was confirmed that the excellent property of its various aspects passes through final sample
SEM image can be found that surface is tightly surrounded by titanium dioxide element, the use of titanium is not only reduced relative to titanium dioxide
Amount, and still remain the optical property of titanium.And silicon titanium valve body is scattered in absolute ethyl alcohol again when sample test, it can
To find that silicon titanium is compound still intact, there is no silica titanium key is destroyed, its stability is further demonstrated.Sample is carried out later
Energy dispersion X-ray spectrometer analysis, it was confirmed that element species and ratio during our silicon titaniums are compound.
Transformation in order to detect its crystal form has carried out XRD tests to titanium dioxide in sample, it can be found that most of dioxy
Change titanium and have been converted into rutile-type, since rutile-type product crystal form is more towards hexahedron, compares anatase and be easier to disperse
Uniformly, it is more uniform to be formed by composite granule, it is made to be more applicable for various building coatings, industrial paint, anti-decaying paint, oil
The industries such as ink, powdery paints.
The most important coloration to silicon titanium composite granule has carried out the test of comprehensive profession, first by being compared with titanium dioxide
First I most directly can be found that the aberration of titanium dioxide is that 3.08 to be apparently higher than our silicon titanium ratios be 2 by CMC tolerance methods:1 sample
The 1.62 of product, it was confirmed that the whiteness of our samples is fully achieved or even has surmounted the brightness levels of titanium dioxide, secondly other aberration
L* brightness values, a* red greens value, b* yellow blues value, C* intensity values, h ° of hue angle angle value are all significantly less than the relative number of titanium dioxide
Value, the whiteness for further demonstrating sample fully achieve titanium dioxide in the Colorimetry formula that National Bureau of Standards is released
NBS aberration 0.00~0.50 (small aberration) correspondence whiteness.We are compared different proportion coloration, are found big
About silicon titanium ratio is 4:Basic and titanium dioxide CMC tolerance method aberration is suitable when 1.
Claims (4)
1. a kind of preparation method of silicon titanium composite granule, which is characterized in that include the following steps：
Step 1：Prepare the dispersion liquid of active micro silicon powder
By surface contain great amount of hydroxy group and form hydrophilic silicon powder i.e. active micro silicon powder and be scattered in absolute ethyl alcohol；
Step 2：The preparation of nanoscale titanium hydroxide colloidal sol
Under stirring conditions by butyl titanate, to the continuous spray water in its surface and the mixed solution for slowing down agent, make butyl titanate
Complete hydrolysis, therein to slow down agent be that can slow down the reagent of butyl titanate hydrolysis rate；
Step 3：Final silicon titanium is compound
Nano level titanium dioxide prepared by the dispersion liquid and step 2 of the active micro silicon powder finally prepared by above-mentioned steps one
It carries out compound, two kinds of samples is put into high speed agitator and are mixed, carrying out at least one hour high-speed stirred keeps its compound uniformly, it
Deposition incubation one hour afterwards, the titanium hydroxide Sol-gel Coated that the titania sources compound such as butyl titanate is formed after hydrolyzing is lived
Property silicon powder particle surface, deposit incubation after, carry out centrifugal solid-liquid separation, later pass through 800 DEG C of -900 DEG C of high temperature it is lazy
Property gas in roasting be high temperature inert atmosphere heat treatment dehydration structure silica titanium key, the titanium dioxide crystal form being formed simultaneously is converted to
Rutile-type forms the silicon dioxide composite powder of rutile titanium dioxide cladding.
2. a kind of preparation method of silicon titanium composite granule described in accordance with the claim 1, which is characterized in that step 1 is lived per 5kg
Property silicon powder corresponds to 5-15L absolute ethyl alcohols.
3. a kind of preparation method of silicon titanium composite granule described in accordance with the claim 1, which is characterized in that when silicon titanium composite granule
Middle silicon titanium molar ratio is (1-4)：1.
4. a kind of silicon titanium composite granule being prepared according to claim 1-3 any one of them methods.
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Cited By (1)
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| CN115260845A (en) * | 2022-09-02 | 2022-11-01 | 中国江西国际经济技术合作有限公司 | Anti-aging processing method for building construction bearing structure |
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