CN106752110A - A kind of preparation method of TiO 2 pigment used for decorative paper - Google Patents
A kind of preparation method of TiO 2 pigment used for decorative paper Download PDFInfo
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- CN106752110A CN106752110A CN201611028312.9A CN201611028312A CN106752110A CN 106752110 A CN106752110 A CN 106752110A CN 201611028312 A CN201611028312 A CN 201611028312A CN 106752110 A CN106752110 A CN 106752110A
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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
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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
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/3623—Grinding
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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
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- 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
- C09C1/3661—Coating
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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
- C09C3/006—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
- C09C3/041—Grinding
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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
- C09C3/063—Coating
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/28—Colorants ; Pigments or opacifying agents
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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
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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
- C01P2006/90—Other properties not specified above
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- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides a kind of preparation method of TiO 2 pigment used for decorative paper, ground after silicate and rutile titanium dioxide slurry are mixed, obtain mixed slurry；The mixed slurry that will be obtained mixes with water-soluble cerium salt, adjusts pH value, and maturation process first is carried out after obtaining alkaline slurry；The product of maturation process first that will be obtained mixes with silicate solutions, carries out second maturation process；Second maturation process product will be obtained to mix with aluminum contained compound, pH value will be adjusted, third time maturation process will be carried out after obtaining the mixed slurry that pH value is 7~9；Third time maturation process product will be obtained to mix with aluminum contained compound, regulation pH value, the 4th maturation process is carried out after obtaining the mixed slurry that pH value is 5~7, the preparation method that obtains the TiO 2 pigment used for decorative paper that the TiO 2 pigment used for decorative paper present invention is provided is simple to operate, low cost, and the TiO 2 pigment for preparing has high-light-fastness, high covering power and good retention.
Description
Technical field
The present invention relates to pigment technology field, more particularly to a kind of preparation method of TiO 2 pigment used for decorative paper.
Background technology
Titanium dioxide turns into best Chinese white with its excellent optical property, is widely used in paper industry, and
Facing paper industry is titanium dioxide main application industry in field of papermaking, and facing paper is called laminated paper, is mainly used in wood-based plate
Veneer, facing paper is very high to pigment light resistance index request, but titanium dioxide has certain defect as Chinese white,
Due to there are many photoactivation points on titanium dioxide surface, under the action of uv light, the oxonium ion on its lattice can lose two
Individual electronics is changed into oxygen atom, and the electronics released is captured by tetravalence titanium ion, is reduced into trivalent titanium ion, and reaction is released
Activity hydroxy and hydroperoxyl free radical, the activity with height can make around titanium dioxide organic polymer oxidation, drop
, there are the breakoff phenomenons such as loss of gloss, discoloration in solution.Therefore, the improvement of the photoactivity of TiO 2 pigment is received significant attention.
Frequently with adding alchlor in oxidizing process during prior art chloridising production TiO 2 pigment, and
All kinds of inorganic hydrous oxides, such as silica, zirconium oxide, aluminum oxide, cerium oxide, five phosphorous oxides are introduced in aftertreatment technology
To suppress the photochemical activity of titanium dioxide, to improve its light fastness in application process, but production technology is tediously long, production
Efficiency is low, and zirconates is a kind of expensive raw material, increased the manufacturing cost of TiO 2 pigment.Such as Chinese patent
CN104179066A discloses a kind of production method of decorative laminate rutile titanium dioxide pigment, by titanium dioxide
Surface of pigments first coats one layer of silicon compound, then coats one layer of aluminium compound, so as to improve the weatherability of TiO 2 pigment,
And the hydroxyl on clad is removed by way of calcining heating, it is to avoid the reaction of electronics pair, but calcining heating is a large amount of by consumption
Energy.
The content of the invention
It is an object of the invention to provide a kind of preparation method of TiO 2 pigment used for decorative paper, the method operation letter
Single, low cost, the TiO 2 pigment for preparing has high-light-fastness, high covering power and good retention.
The invention provides a kind of preparation method of TiO 2 pigment used for decorative paper, comprise the following steps：
(1) ground after mixing silicate and rutile titanium dioxide slurry, obtain mixed slurry；
(2) mixed slurry for obtaining the step (1) mixes with water-soluble cerium salt, adjusts pH value, obtains alkaline slurry
After carry out maturation process first；
(3) product of maturation process first for obtaining the step (2) mixes with silicate, and regulation pH value is entered to 6~7
Second maturation process of row；
(4) step (3) is obtained into second maturation process product to mix with aluminum contained compound, regulation pH value to 5~
7, the mixed slurry that will be obtained carries out third time maturation process, obtains TiO 2 pigment used for decorative paper.
Preferably, the solvent in step (1) the rutile titanium dioxide slurry is deionized water, the rutile-type
The concentration of titania slurry is (250~400) g/L.
Preferably, in the step (2), the temperature of the mixed slurry mixed with water-soluble cerium salt is 50~90 DEG C.
Preferably, the quality of step (2) the water-soluble cerium salt, with cerium oxide, is the rutile titanium dioxide
The 0.5%~1.0% of the quality of middle titanium dioxide.
Preferably, step (2) the water-soluble cerium salt is added in the form of water-soluble cerium solution；
The concentration of the water-soluble cerium solution is calculated as (50~100) g/L with the content of ceria.
Preferably, the quality of silicate is the rutile-type dioxy in terms of the quality of silica in the step (3)
Change the 2.0%~4.0% of the quality of titanium dioxide in titanium.
Preferably, the silicate in the step (3) is added in the form of silicate solutions；
The concentration of the silicate solutions is calculated as (50~200) g/L with the content of silica.
Preferably, the quality of aluminum contained compound is the rutile-type dioxy in terms of alundum (Al2O3) in the step (4)
Change the 1.0%~3.0% of the quality of titanium dioxide in titanium.
Preferably, step (4) aluminum contained compound is added in the form of aluminum contained compound solution；
The concentration of the aluminum contained compound solution is calculated as (80~200) g/L with the content of alundum (Al2O3).
Preferably, the conditioning agent that regulation pH value is used in the step (4) is inorganic acid solution or acidic salt solution.
The invention provides a kind of preparation method of TiO 2 pigment used for decorative paper, by silicate and rutile-type dioxy
Ground after changing the mixing of titanium slurry, obtain mixed slurry；The mixed slurry that will be obtained mixes with water-soluble cerium salt, adjusts pH value, obtains
Maturation process first is carried out after to alkaline slurry；The product of maturation process first that will be obtained mixes with silicate, regulation pH value to 6
~7, carry out second maturation process；Second maturation process product will be obtained to mix with aluminum contained compound, regulation pH value to 5~
7, the mixed slurry that will be obtained carries out third time maturation process, obtains TiO 2 pigment used for decorative paper.
The present invention is by the dispersion and milled processed using silicate to rutile titanium dioxide slurry, it is ensured that starched before coating
Material particle exists with the form of initial size, so that the hydrous ceria continuous uniform of cladding；By adding water-soluble cerium salt
Solution and maintain slurry pH value for alkalescence, it is ensured that on titanium dioxide surface formed continuous uniform hydrous ceria clad,
It is to utilize Ce to coat this coating film4+/Ce3+Oxidation reduction electro-dynamic potential be higher than Ti4+/Ti3+Oxidation reduction electro-dynamic potential, having Ce4 +In the presence of, Ti4+Ti would not be reduced to3+, therefore improve the light fastness of TiO 2 pigment pigment；Obtain aqua oxidation
After cerium clad, add silicate and form silica clad, be that coating again for aqua oxidation aluminium lamination provides more hydroxyls,
It is follow-up that one layer of hydrated alumina clad of densification is coated on silica clad under faintly acid or neutrallty condition, such
The aluminum oxide of type is netted or banded structure, is conducive to improving dispersive property of the TiO 2 pigment pigment in water, Jin Erti
The retention of TiO 2 pigment high.The present invention provide TiO 2 pigment used for decorative paper preparation method it is simple to operate, into
This is low, and the TiO 2 pigment for preparing has high-light-fastness, high covering power and good retention.Test result indicate that,
The TiO 2 pigment of the laminated paper board that the TiO 2 pigment prepared according to technical solution of the present invention is prepared is kept
Rate is above 99.30, and light resistance reaches 0.48~0.97.
Other, rutile-type titanium dioxide in the rutile titanium dioxide that the chlorination that the present invention is used is prepared
Ti content is more than 99%, it is ensured that the covering power of product and basic light fastness.
Specific embodiment
The invention provides a kind of preparation method of TiO 2 pigment used for decorative paper, comprise the following steps：
(1) ground after mixing silicate and rutile titanium dioxide slurry, obtain mixed slurry；
(2) mixed slurry for obtaining the step (1) mixes with water-soluble cerium salt, adjusts pH value, obtains alkaline slurry
After carry out maturation process first；
(3) product of maturation process first for obtaining the step (2) mixes with silicate, and regulation pH value is entered to 6~7
Second maturation process of row；
(4) step (3) is obtained into second maturation process product to mix with aluminum contained compound, regulation pH value to 5~
7, the mixed slurry that will be obtained carries out third time maturation process, obtains TiO 2 pigment used for decorative paper.
The present invention grinds after mixing silicate and rutile titanium dioxide slurry, obtains mixed slurry.In the present invention
In, the solvent in the rutile titanium dioxide slurry is preferably deionized water；The rutile titanium dioxide is preferably by chlorination
Method is prepared.In the present invention, the mass content of rutile titanium dioxide preferably exists in the rutile titanium dioxide
More than 99%.The present invention does not have particular/special requirement to the chloridising, using well-known to those skilled in the art for titanium dioxide
Chloridising prepared by titanium.In the present invention, the concentration of the rutile titanium dioxide slurry is preferably (250~400)
G/L, more preferably (300~350) g/L, most preferably 320g/L.
In the present invention, when silicate and rutile titanium dioxide slurry mix, the consumption of the silicate is with dioxy
The quality meter of SiClx, is the 1.0%~3.0% of the quality of titanium dioxide in the rutile titanium dioxide, further preferably
It is 1.5 ‰~2.5 ‰, most preferably 2 ‰.
In the present invention, the silicate is added preferably in the form of silicate solutions；It is molten in the silicate solutions
Agent is preferably deionized water.In the present invention, the concentration of the concentration silicate solutions of the silicate solutions is with silica
Content meter, preferably (50~200) g/L, more preferably (75~150) g/L, most preferably 100g/L.In the present invention,
The silicate is preferably sodium metasilicate and/or potassium silicate.
Mode present invention preferably employs stirring completes the mixing of the silicate and rutile titanium dioxide slurry, this
Invention does not have particular/special requirement to the mode of the stirring, using agitating mode well-known to those skilled in the art.This hair
It is bright, the dispersion between the silicate and the rutile titanium dioxide slurry can be promoted in the whipping process, it is easy to
The uniformity of particle in follow-up process of lapping.
After the present invention completes the mixing of the silicate and rutile titanium dioxide slurry, it is ground.In the present invention
In, the particle diameter of mixed slurry is preferably 150~250nm, more preferably 160~225nm after the grinding.The present invention is to institute
The no particular/special requirement of grinding is stated, uses the mode of grinding well-known to those skilled in the art to obtain the mixing of target size
Slurry.
Mixed slurry after the grinding is preferably warming up to 50~90 DEG C by the present invention, more preferably 55~75 DEG C,
Most preferably 60 DEG C.Subsequent reactions of the present invention are carried out under preferably remaining in the temperature after the intensification.
After obtaining mixed slurry, the present invention mixes the mixed slurry with water-soluble cerium salt, adjusts pH value, obtains alkalescence
Maturation process first is carried out after slurry.In the present invention, the addition of the water-soluble cerium salt is with cerium oxide, preferably institute
State the 0.5%~1.0% of the quality of titanium dioxide in rutile titanium dioxide, more preferably 0.3%~0.4%.
In the present invention, the water-soluble cerium salt is preferably cerous sulfate or cerous nitrate.
In the present invention, the water-soluble cerium salt is added preferably in the form of water-soluble cerium solution.In the present invention, institute
The concentration of water-soluble cerium solution is stated with the content meter of ceria, preferably (50~100) g/L, more preferably (60~
80)g/L.Preferably be added to the water-soluble cerium solution in the mixed slurry obtained after the grinding by the present invention；In this hair
In bright, the addition time of the water-soluble cerium solution is preferably 0.5~1.0h, more preferably 0.75~0.9h, optimal
Elect 0.8h as.
After completing the mixed slurry and the mixing of the water-soluble cerium salt, the pH value of present invention regulation feed liquid to alkalescence,
Obtain alkaline slurry.In the present invention, the conditioning agent for adjusting the pH value is preferably inorganic alkali solution or alkaline salt solution.At this
In invention, the pH value of the alkaline slurry is preferably 8.0~9.5, more preferably 8.8~9.0.The present invention is to described inorganic
The no particular/special requirement in source of aqueous slkali or alkaline salt solution, using inorganic alkali solution well-known to those skilled in the art or alkali
Property salting liquid, in an embodiment of the present invention, the inorganic alkali solution specifically use sodium hydroxide solution or potassium hydroxide
Solution；The alkaline salt solution is specifically using in sodium carbonate liquor, solution of potassium carbonate, sodium aluminate solution and potassium metaaluminate solution
One or more.
After obtaining alkaline slurry, the alkaline slurry is carried out maturation process first by the present invention.In the present invention, the head
Secondary maturation process is preferably carried out under agitation, and the time of the maturation process first is preferably 10~60min, further excellent
Elect 20~30min as.In the present invention, the frequency of the stirring is preferably 100~150rpm, more preferably 120~
130rpm.The present invention does not have particular/special requirement to the specific embodiment of the stirring, using well-known to those skilled in the art
Agitating mode.In the present invention, during the maturation process first, formed on the rutile titanium dioxide surface
The clad of hydrous ceria first.
First after maturation process, maturation process product mixes the present invention with silicate first by described in, and regulation pH value to 6~
7, carry out second maturation process.In the present invention, during second maturation process, the quality of silicate is with the quality of silica
Meter, the 2.0%~4.0% of the quality of titanium dioxide, more preferably 2.5% in preferably described rutile titanium dioxide
~3.5%, most preferably 3%.In the present invention, the silicate is added preferably in the form of silicate solutions；In the present invention
In, the concentration of the silicate solutions is with the content meter of silica, preferably (50~200) g/L, more preferably (100
~150) g/L.During the silicate solutions are preferably added the product after the maturation process first by the present invention, the completion head
The mixing of secondary maturation process product and silicate solutions；In the present invention, the addition time of the silicate solutions be preferably 10
~30min, more preferably 15~20min.
In the present invention, the product of maturation process first and the pH value of the mixed slurry of silicate are 6~7, enter one
Step is preferably 6.1~6.9, more preferably 6.5~6.6.In the present invention, the conditioning agent for adjusting the pH value is preferably inorganic acid
Or acidic salt solution.The no particular/special requirement in source to the inorganic acid or acidic salt solution of the invention, using art technology
Inorganic acid or acidic salt solution known to personnel, in an embodiment of the present invention, the inorganic acid-specific using hydrochloric acid,
One or more in sulfuric acid and nitric acid；The acidic salt solution specifically uses sodium aluminate solution or potassium metaaluminate solution.
In the present invention, second maturation process is preferably carried out under agitation, the present invention to the stirring at
No particular/special requirement is managed, using agitating mode well-known to those skilled in the art；In the present invention, it is described ripe for the second time
The time for changing treatment is preferably 1~2h, more preferably 1.5~1.8h.In the present invention, the frequency of the stirring is preferably
200~250rpm, more preferably 230~240rpm.
After second maturation process, the present invention will obtain second maturation process product and mix with aluminum contained compound, regulation
PH value, third time maturation process is carried out after obtaining the mixed slurry that pH value is 6~7.In the present invention, the aluminum contained compound is excellent
Elect aluminium salt and/or meta-aluminate as；The aluminium salt is preferably aluminum sulfate and/or alchlor in the present invention；In the present invention,
The meta-aluminate is preferably sodium metaaluminate and/or potassium metaaluminate.In the present invention, the addition of the aluminum contained compound is with three
Al 2 O meter, the 1.0%~3.0% of the quality of titanium dioxide in preferably described rutile titanium dioxide is further excellent
Elect 1.5%~2.0% as.In the present invention, the aluminum contained compound is added preferably in the form of aluminum contained compound solution；At this
In invention, the concentration of the aluminum contained compound solution with the content meter of aluminium, preferably (1.5~4.0) mol/L, further preferably
It is (2.0~3.0) mol/L, most preferably 2.5mol/L.The aluminum contained compound solution is preferably added described second by the present invention
In product after secondary maturation process, the mixing of second maturation process product and aluminum contained compound solution is completed；In this hair
In bright, the addition time of the aluminum contained compound solution is preferably 1~2h, more preferably 1.2~1.4h.
After the mixing of second maturation process product and aluminum contained compound, the pH value for adjusting feed liquid of the invention to 6~
7.In the present invention, the conditioning agent for adjusting the pH value use is preferably inorganic acid solution or acidic salt solution.In the present invention,
The pH value of the feed liquid that second maturation process product is mixed to get with aluminum contained compound is preferably 6.2~6.5.
In the present invention, the inorganic acid solution is preferably one or more in hydrochloric acid, sulfuric acid and nitric acid；The acidity
Salting liquid is preferably aluminum sulfate solution and/or aluminum trichloride solution.In the present invention, the inorganic acid solution, acidic salt solution,
The concentration of inorganic alkali solution and alkaline salt solution is preferably independently 10~20mol/L, more preferably 15~18mol/L.
After obtaining the feed liquid that pH value is 6~7, the present invention carries out at third time curing the feed liquid that the pH value is 6~7
Reason.In the present invention, the third time maturation process is preferably carried out under agitation, and the present invention does not have to the stir process
Particular/special requirement, using agitating mode well-known to those skilled in the art；In the present invention, the third time maturation process
Time be preferably 1~2h, more preferably 1.5~1.8h.In the present invention, the frequency of the stirring be preferably 50~
120rpm, more preferably 80~90rpm.The present invention does not have particular/special requirement to the specific embodiment of the stirring, uses
Agitating mode well-known to those skilled in the art.
After obtaining hydrous ceria clad, add silicate and form silica clad, be aqua oxidation aluminium lamination
The more hydroxyls of offer are provided again, subsequently under faintly acid or neutrallty condition, one layer of densification of cladding on silica clad
Hydrated alumina clad, the aluminum oxide of the type is netted or banded structure, is conducive to raising TiO 2 pigment pigment to exist
Dispersive property in water, and then improve the retention of TiO 2 pigment.
In the present invention, during the third time maturation process, under faintly acid or neutrallty condition, in p chloromethylbenzoic acid oxygen oxygen
One layer of clad of the hydrated alumina of densification the 3rd is coated on SiClx clad, the aluminum oxide of the type is netted or banding knot
Structure, is conducive to improving dispersive property of the TiO 2 pigment pigment in water.
In the present invention, it is preferably in titanium dioxide table according to the TiO 2 pigment prepared in above-mentioned technical proposal
Face is coated with the particle of hydrous ceria clad, silica clad and hydrated alumina clad successively.In the present invention,
The particle diameter of the TiO 2 pigment is preferably 10~50nm, more preferably 15~30nm.
After the third time maturation process, the present invention is preferably washed the product after the third time maturation process successively
Wash, dry, air-flow crushing and gas solid separation, obtain TiO 2 pigment used for decorative paper.
In the present invention, the washing is preferably carried out using deionized water；In the present invention, the temperature of the deionized water
Preferably 50~80 DEG C, most preferably more preferably 55~75 DEG C, 60 DEG C.The present invention is not special to the wash time
It is required that, the resistivity of the filter cake to obtain is defined more than 10000 Ω cm, the resistivity further preferred 12000 of the filter cake
~20000 Ω cm.
The present invention does not have particular/special requirement to the drying, air-flow crushing and gas solid separation, using those skilled in the art institute
Well known technical scheme.In the present invention, the air-flow crushing improves TiO 2 pigment dispersiveness.
The invention provides a kind of preparation method of TiO 2 pigment used for decorative paper, by silicate and rutile-type dioxy
Ground after changing the mixing of titanium slurry, obtain mixed slurry；The mixed slurry that will be obtained mixes with water-soluble cerium salt, adjusts pH value, obtains
Maturation process first is carried out after to alkaline slurry；The product of maturation process first that will be obtained mixes with silicate, regulation pH value to 6
~7, carry out second maturation process；Second maturation process product will be obtained to mix with aluminum contained compound, regulation pH value to 5~
7, the mixed slurry that will be obtained carries out third time maturation process, obtains TiO 2 pigment used for decorative paper.
The present invention is by the dispersion and milled processed using silicate to rutile titanium dioxide slurry, it is ensured that starched before coating
Material particle exists with the form of initial size, so that the hydrous ceria continuous uniform of cladding；By adding water-soluble cerium salt
Solution and maintain slurry pH value for alkalescence, it is ensured that on titanium dioxide surface formed continuous uniform hydrous ceria clad,
It is to utilize Ce to coat this coating film4+/Ce3+Oxidation reduction electro-dynamic potential be higher than Ti4+/Ti3+Oxidation reduction electro-dynamic potential, having Ce4 +In the presence of, Ti4+Ti would not be reduced to3+, therefore improve the light fastness of TiO 2 pigment pigment；Obtain aqua oxidation
After cerium clad, add silicate and form silica clad silica clad, be that coating again for aqua oxidation aluminium lamination carries
For more hydroxyls, subsequently under faintly acid or neutrallty condition, one layer of aqua oxidation of densification is coated on silica clad
Aluminium clad, the aluminum oxide of the type is netted or banded structure, be conducive to improve TiO 2 pigment pigment in water point
Performance is dissipated, and then improves the retention of TiO 2 pigment.The preparation side of the TiO 2 pigment used for decorative paper that the present invention is provided
Method is simple to operate, low cost, and the TiO 2 pigment for preparing has high-light-fastness, high covering power and good retention.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.It is aobvious
So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the reality in the present invention
Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made all belongs to
In the scope of protection of the invention.
Embodiment 1
(1) the rutile titanium dioxide first product powder 500g that chloridising is prepared, wherein rutile-type dioxy are weighed
Rutile content adds deionized water to be configured to the slurry of 250g/L more than 99% in changing titanium first product, adds with SiO2Account for
TiO in first product2Weight is calculated as 1 ‰ sodium silicate solution, and the concentration of sodium silicate solution is with SiO250g/L is calculated as, stirring is disperseed
Treatment, is then ground, and grinding disposed slurry average grain diameter is 160nm；
(2) slurry after sand milling is warming up to 50 DEG C, and whole coating process is maintained this temperature.
(3) added with CeO in 0.5h2With TiO in first product2The cerous nitrate solution of the 0.5% of quality, wherein cerous nitrate are molten
The concentration of liquid is with CeO250g/L is calculated as, while maintaining slurry pH between 8.0~8.2 with sodium hydroxide solution, stirring is cured
10min, the clad of hydrous ceria first is formed in titanium dioxide surface.
(4) added with SiO in 10min2Account for TiO in first product2Weight is calculated as 2.0% sodium silicate solution, sodium silicate solution
Concentration is with SiO250g/L is calculated as, adds sulfuric acid to maintain slurry pH value in 6.0~6.2, stirring curing 1h, on the first clad
Form the second clad silicon clad.
(5) added with Al in 0.5h2O3With TiO in first product2The sodium aluminate solution of the 3.0% of quality, wherein meta-aluminic acid
Sodium solution concentration is with Al2O380g/L is calculated as, adds 20wt% sulfuric acid to maintain slurry pH value between 5.5~5.7, stirring is cured
1h, forms the clad of hydrated alumina the 3rd on the second clad.
(6) the Ω cm of filter cake resistivity 11000 are washed till with 50 DEG C of deionized waters, then be dried, air-flow crushing, by gas
Gu separation and recovery, obtains titanium dioxide pigment special for laminated paper pigment.
Embodiment 2
(1) the rutile titanium dioxide first product powder 600g that chloridising is prepared, wherein rutile-type dioxy are weighed
Rutile content adds deionized water to be configured to the slurry of 300g/L more than 99% in changing titanium first product, adds with SiO2Account for
TiO in first product2Weight is calculated as 2 ‰ sodium silicate solution, and the concentration of sodium silicate solution is with SiO2100g/L is calculated as, stirring is divided
Treatment is dissipated, is then ground, grinding disposed slurry average grain diameter is 210nm；
(2) slurry after sand milling is warming up to 70 DEG C, and whole coating process is maintained this temperature.
(3) added with CeO in 0.5h2With TiO in first product2The cerous sulfate solution of the 0.7% of quality, cerous sulfate solution
Concentration is with CeO270g/L is calculated as, while maintaining slurry pH between 8.8~9.0 with potassium hydroxide solution, stirring cures 30min,
The clad of hydrous ceria first is formed in titanium dioxide surface.
(4) added with SiO in 20min2Account for TiO in first product2Weight is calculated as 3.0% sodium silicate solution, silicate solutions
Concentration is with SiO2100g/L is calculated as, adds the sulfuric acid that mass fraction is 20% to maintain slurry pH value between 6.4~6.6, stirred
Curing 1.5h, forms the second clad silicon clad on the first clad.
(5) added with Al in 1.0h2O3With TiO in first product2The aluminum sulfate solution of the 1.5% of quality, aluminum sulfate solution is dense
Degree is with Al2O3120g/L is calculated as, slurry pH value is maintained between 6.0~6.2, stirring curing 2h forms water on the second clad
Close the clad of aluminum oxide the 3rd.
(6) the Ω cm of filter cake resistivity 12000 are washed till with 60 DEG C of deionized waters, then be dried, air-flow crushing, by gas
Gu separation and recovery, obtains titanium dioxide pigment special for laminated paper pigment.
Embodiment 3
(1) the rutile titanium dioxide first product powder 800g that chloridising is prepared, wherein rutile-type dioxy are weighed
Rutile content adds deionized water to be configured to the slurry of 400g/L more than 99% in changing titanium first product, adds with SiO2Account for
TiO in first product2Weight is calculated as 3 ‰ silicate solutions, and the concentration of silicate solutions is with P2O5200g/L is calculated as, stirring is divided
Treatment is dissipated, is then ground, grinding disposed slurry average grain diameter is 250nm；
(2) slurry after sand milling is warming up to 90 DEG C, and whole coating process is maintained this temperature.
(3) added with CeO in 1.0h2With TiO in first product2The cerous nitrate solution of the 1.0% of quality, wherein cerous nitrate are molten
The concentration of liquid is with CeO2100g/L is calculated as, while maintaining slurry pH between 9.2~9.5 with sodium hydroxide solution, stirring is cured
60min, the clad of hydrous ceria first is formed in titanium dioxide surface.
(4) added with SiO in 30min2Account for TiO in first product2Weight is calculated as 4.0% potassium silicate solution, potassium silicate solution
Concentration is with SiO250g/L is calculated as, adds the sulfuric acid that mass fraction is 20% to maintain slurry pH value between 6.8~7.0, stirred ripe
Change 2h, the second clad silicon clad is formed on the first clad.
(5) added with Al in 2.0h2O3With TiO in first product23.0% potassium metaaluminate solution of quality, potassium metaaluminate solution
Concentration is with Al2O3200g/L is calculated as, is added with Al2O3The aluminum sulfate solution for being calculated as 100g/L maintains slurry pH value 6.8~7.0
Between, stirring curing 3h forms the clad of hydrated alumina the 3rd on the second clad.
(6) the Ω cm of filter cake resistivity 16000 are washed till with 80 DEG C of deionized waters, then be dried, air-flow crushing, by gas
Gu separation and recovery, obtains titanium dioxide pigment special for laminated paper pigment.
Embodiment 4
(1) the rutile titanium dioxide first product powder 800g that chloridising is prepared, wherein rutile-type dioxy are weighed
Rutile content adds deionized water to be configured to the slurry of 400g/L more than 99% in changing titanium first product, adds with SiO2Account for
TiO in first product2Weight is calculated as 3 ‰ silicate solutions, and the concentration of silicate solutions is with P2O5200g/L is calculated as, stirring is divided
Treatment is dissipated, is then ground, grinding disposed slurry average grain diameter is 250nm；
(2) slurry after sand milling is warming up to 90 DEG C, and whole coating process is maintained this temperature.
(3) added with CeO in 1.0h2With TiO in first product2The cerous sulfate solution of the 1.0% of quality, wherein cerous sulfate is molten
The concentration of liquid is with CeO2100g/L is calculated as, while maintaining slurry pH between 9.2~9.5 with potassium hydroxide solution, stirring is cured
60min, the clad of hydrous ceria first is formed in titanium dioxide surface.
(4) added with SiO in 30min2Account for TiO in first product2Weight is calculated as 4.0% potassium silicate solution, potassium silicate solution
Concentration is with SiO250g/L is calculated as, adds the sulfuric acid that mass fraction is 20% to maintain slurry pH value between 6.8~7.0, stirred ripe
Change 2h, the second clad silicon clad is formed on the first clad.
(5) added with Al in 2.0h2O3With TiO in first product23.0% aluminum sulfate solution of quality, aluminum sulfate solution concentration
With Al2O3200g/L is calculated as, is added with Al2O3Be calculated as 100g/L aluminum trichloride solution maintain slurry pH value 6.8~7.0 it
Between, stirring curing 3h forms the clad of hydrated alumina the 3rd on the second clad.
(6) the Ω cm of filter cake resistivity 16000 are washed till with 80 DEG C of deionized waters, then be dried, air-flow crushing, by gas
Gu separation and recovery, obtains titanium dioxide pigment special for laminated paper pigment.
Reference examples 1
The inorganic process step of embodiment 1 is repeated, cancels step 3 and step 4 in embodiment 1.
Reference examples 2
The inorganic process step of embodiment 1 is repeated, cancels step 4, step 5 and step 6 in embodiment 1.
Laminated paper board progressive is made to TiO 2 pigment pigment prepared by above-described embodiment 1~4 and reference examples 1~2
Can detect, wherein obtaining L, a, b using GB/T5211.20-1999 (chromatmetry) detections, (what L, a, b three respectively represents and join
Number)；Light resistance Δ E is determined in ultraviolet (UVA) light irradiation 5h；And TiO 2 pigment retention method of testing：Take 5g finished products two
After titanium oxide pigments and 300g paper pulp mix with 500mL water high-speed stirreds, filtering copy paper is carried out, paper is dried, be placed in constant weight
Crucible in calcination, measurement ash content after calculate retention.Testing result is as shown in table 1.
The TiO 2 pigment of table 1 is made laminated paper board contrasting detection result
By the data in table 1 can be seen that according to the present invention production TiO 2 pigment have excellent photostability,
Covering power, easily disperse and good retention.
Δ E refers to the chromatic aberration after pre-irradiation in table 1, and chromatic aberration is smaller, illustrates that light resistance is better.L*, A*, B* are states
The characteristic index of the general TiO 2 pigment whiteness in border, L* refers to brightness, and A* refers to the greenish-yellow value of color, and B* refers to that the indigo plant of color is yellow
Value, L*, A*, B* mainly have direct relation with the particle diameter of TiO 2 pigment, and L*, A*, B* numerical value change are shown in table 1 less,
Show that the particle diameter of the TiO 2 pigment after the TiO 2 pigment of non-coating and coating is more or less the same；But with air after coating
And the medium of light directly contact changes, titanium dioxide directly contact during non-coating is coating film and air after coating
With light directly contact, the Δ E of the TiO 2 pigment obtained according to technical solution of the present invention is significantly less than and obtained according to comparative example
To the Δ E of uncoated TiO 2 pigment, chromatic aberration is smaller after illustrating coating, and coating effect is better.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of TiO 2 pigment used for decorative paper, comprises the following steps：
(1) ground after mixing silicate and rutile titanium dioxide slurry, obtain mixed slurry；
(2) mixed slurry for obtaining the step (1) mixes with water-soluble cerium salt, adjusts pH value, obtains alkaline slurry laggard
Capable maturation process first；
(3) product of maturation process first for obtaining the step (2) mixes with silicate, and regulation pH value carries out the to 6~7
Post cure treatment；
(4) step (3) is obtained into second maturation process product to mix with aluminum contained compound, regulation pH value to 5~7, will
The mixed slurry for obtaining carries out third time maturation process, obtains TiO 2 pigment used for decorative paper.
2. preparation method according to claim 1, it is characterised in that step (1) the rutile titanium dioxide slurry
In solvent be deionized water, the concentration of the rutile titanium dioxide slurry is (250~400) g/L.
3. preparation method according to claim 1, it is characterised in that in the step (2), mix with water-soluble cerium salt
The temperature of mixed slurry is 50~90 DEG C.
4. the preparation method according to claim 1 or 3, it is characterised in that the quality of step (2) the water-soluble cerium salt with
Cerium oxide, is the 0.5%~1.0% of the quality of titanium dioxide in the rutile titanium dioxide.
5. preparation method according to claim 4, it is characterised in that step (2) the water-soluble cerium salt is with water-soluble cerium
The form of salting liquid is added；
The concentration of the water-soluble cerium solution is calculated as (50~100) g/L with the content of ceria.
6. preparation method according to claim 1, it is characterised in that the quality of silicate is with dioxy in the step (3)
The quality meter of SiClx, is the 2.0%~4.0% of the quality of titanium dioxide in the rutile titanium dioxide.
7. preparation method according to claim 6, it is characterised in that the silicate in the step (3) is molten with silicate
The form of liquid is added；
The concentration of the silicate solutions is calculated as (50~200) g/L with the content of silica.
8. preparation method according to claim 1, it is characterised in that in the step (4) quality of aluminum contained compound with
Alundum (Al2O3) meter, is the 1.0%~3.0% of the quality of titanium dioxide in the rutile titanium dioxide.
9. preparation method according to claim 8, it is characterised in that step (4) aluminum contained compound is closed with containing calorize
The form of thing solution is added；
The concentration of the aluminum contained compound solution is calculated as (80~200) g/L with the content of alundum (Al2O3).
10. the preparation method according to claim 1 or 8, it is characterised in that regulation pH value is used in the step (4)
Conditioning agent is inorganic acid solution or acidic salt solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107254197A (en) * | 2017-06-07 | 2017-10-17 | 常州建轩纺织品有限公司 | A kind of preparation method of high retention rate decorative laminate titanium dioxide |
| CN107574711A (en) * | 2017-08-31 | 2018-01-12 | 安徽安纳达钛业股份有限公司 | A kind of production method of titanium dioxide used for decorative paper |
| CN108929574A (en) * | 2018-09-08 | 2018-12-04 | 江苏中研创星材料科技有限公司 | A kind of preparation method of the dedicated high-grade titanium dioxide of papermaking |
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2016
- 2016-11-18 CN CN201611028312.9A patent/CN106752110A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107254197A (en) * | 2017-06-07 | 2017-10-17 | 常州建轩纺织品有限公司 | A kind of preparation method of high retention rate decorative laminate titanium dioxide |
| CN107574711A (en) * | 2017-08-31 | 2018-01-12 | 安徽安纳达钛业股份有限公司 | A kind of production method of titanium dioxide used for decorative paper |
| CN107574711B (en) * | 2017-08-31 | 2020-01-17 | 安徽安纳达钛业股份有限公司 | Production method of titanium dioxide for decorative paper |
| CN108929574A (en) * | 2018-09-08 | 2018-12-04 | 江苏中研创星材料科技有限公司 | A kind of preparation method of the dedicated high-grade titanium dioxide of papermaking |
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