CN108997788A - The preparation method of high covering power titanium dioxide - Google Patents
The preparation method of high covering power titanium dioxide Download PDFInfo
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention belongs to titanium dioxide production technical fields, and in particular to a kind of preparation method of high covering power titanium dioxide.It need to be improved for the covering power of the titanium white powder coating of existing method preparation, the problems such as preparation process is complicated, at high cost, the present invention provides a kind of preparation method of high covering power titanium dioxide, comprising the following steps: after a, titanium dioxide first product crush plus slurry is made in water;B, slurry is heated, while silicon-containing compound and acid aluminum contained compound is added, cures 30~60min;C, acid aluminum contained compound is added into slurry, cures 30~60min;D, acid aluminum contained compound and alkaline aluminum contained compound is added in cocurrent, reacts 30~60min;E, slurry pH value is adjusted to 7.0~8.5 with alkaline aluminum contained compound, filtering, washing, dry product.The method of the present invention is easy to operate, and the product strong covering power being prepared can save the dosage of titanium dioxide, can be widely applied to the fields such as water paint, matt latex paint, water-based ink.
Description
Technical field
The invention belongs to titanium dioxide production fields, and in particular to a kind of preparation method of high covering power titanium dioxide.
Background technique
Titanium dioxide (TiO2) it is also known as titanium dioxide, it is a kind of white pigment, is often applied to numerous areas, such as coating, modeling
In material, ink, paper and laminate.In TiO2During surface treatment, some chemical substances are added under given conditions
The performance of titanium dioxide, such as covering power, dispersibility can be increased.
Titanium dioxide is as coating in application, the covering power and whiteness of coating are most important.The covering power and titanium white of titanium dioxide
Powder and resin index are only poor related, and difference is bigger, and covering power is higher.Coated fertilizer common at present has silica or oxidation
Aluminium etc..
The refractive index of hydrated SiO 2 is lower, when introducing hydrated SiO 2 in the surface treatment process of titanium dioxide,
The difference of refractive index can be increased, single titanium dioxide particle is isolated to greatest extent, be allowed in good dispersity, and wrapped
Covering a large amount of hydrated SiO 2 can make titanium dioxide surface loose porous, improve the hydrophilicity of titanium dioxide, make titanium dioxide
Covering is more preferable.Equally, in titanium dioxide Coated by Silica~aluminium oxide hydrate, it can also be improved titanium dioxide as water
Property coating application when covering power.
United States Patent (USP) US3510335 discloses a kind of production method of improved titanium dioxide pigment, titanium dioxide~
The silicon dioxide film of aluminium oxide cooxidation object surface of pigments cladding about 1~25%, is then calcined under the conditions of 300~1000 DEG C,
It can get a kind of fastness and the high titanium dioxide covered.
United States Patent (USP) US4075031 discloses a kind of method for improving titanium dioxide pigment covering power, can be in high temperature 90
One layer of fine and close amorphous silica and pellumina are coated under the conditions of DEG C.But since temperature is higher, reaction is not easy this method
Control, deposit cannot be completely deposited on TiO 2 particles, to affect covering and dispersion of titanium dioxide etc.
Performance.
Chinese patent CN1850914A discloses a kind of method for improving titanium dioxide pigment and covering power, by titanium dioxide
One layer of dense oxide silicon is coated at high temperature, then coats loose silicon and pellumina under the conditions of neutral meta-alkalescence, can be improved
The weatherability and covering power of titanium dioxide.But the entire first high temperature of coating process needs, then low temperature, operation difficulty are big;And sulfuric acid is used
Measure it is larger, sulfuric acid can only play the role of during entire coating adjust pH, cause unnecessary waste.
Chinese patent CN101885926A discloses a kind of method for producing rutile type titanium white powder with high hiding power, in high-temperature alkali
Property under the conditions of sodium metasilicate is added, after with sulfuric acid be adjusted to highly acid (pH=0.8~1.5), this method is in the process for adjusting slurry pH
In easily cause that the silicon dioxide film of cladding dissolves again and itself causes cladding not exclusively to influence the covering power of titanium dioxide in core.
The above method can be handled in titanium dioxide surface, change its weatherability or covering power.But it operates
Condition is not easy to control or covering power is poor, this field be badly in need of developing it is a kind of it is easy to operate, production cost is low, strong covering power
The preparation method of high covering power titanium dioxide.
Summary of the invention
The technical problem to be solved in the present invention are as follows: the covering power of the titanium white powder coating of existing method preparation need to be improved,
The problems such as preparation process is complicated, at high cost.
The technical solution of present invention solution above-mentioned technical problem are as follows: a kind of preparation method of high covering power titanium dioxide is provided.
Method includes the following steps:
A, titanium dioxide first product is crushed, adds water that slurry is made, dispersing agent is added, adjusting slurry pH value is 9.0~11.0;
B, the obtained slurry of step a is heated to 40~60 DEG C, while silicon-containing compound and acid aluminum contained compound is added,
Keeping slurry pH value is 8.5~10.5, cures 30~60min;
C, acid aluminum contained compound is added in the slurry obtained to step b, adjusting slurry pH value is 4.0~6.5, curing 30
~60min;
D, acid aluminum contained compound and alkaline aluminum contained compound is added in cocurrent in the slurry obtained to step c, keeps slurry
PH value be 4.5~6.5, cure 30~60min;
E, the slurry pH value obtained by alkaline aluminum contained compound regulating step d is filtered, washing, is obtained after dry to 7.0~8.5
To high covering power titanium dioxide.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, titanium dioxide crude product described in step a refers to through sulfuric acid
Method or the not surface treated titanium dioxide of chloridising production.Preferably rutile titanium dioxide.Further, described two
Ti content is 80~90% in titanium oxide.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, smashed partial size described in step a be 200~
350nm。
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, slurry concentration described in step a be 350g/L~
450g/L。
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, dispersing agent described in step a is sodium metasilicate, hexa metaphosphoric acid
At least one of sodium or monoisopropanolamine, additive amount are to make slurry viscosity 50cp~300cp.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, heating slurry temperature described in step b to 45 DEG C~55
℃。
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, silicon-containing compound additive amount is described in step b with dioxy
SiClx meter is 5.0~15.0% of titanium dioxide quality in slurry.
Preferably, in the preparation method of above-mentioned high covering power titanium dioxide, the dosage of silicon-containing compound described in step b is with two
Silica meter is 6.0~10.0% of titanium dioxide quality in slurry.
Preferably, in the preparation method of above-mentioned high covering power titanium dioxide, silicon-containing compound described in step b be sodium metasilicate or
Potassium silicate, concentration are 280~300g/L.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, the additive amount of aluminum contained compound described in step b is with three
Al 2 O meter is 3.5~10.5% of titanium dioxide quality in slurry.
Preferably, in the preparation method of above-mentioned high covering power titanium dioxide, the additive amount of aluminum contained compound described in step b with
Aluminum oxide meter is 4.2~7.0% of titanium dioxide quality in slurry.
Specifically, in the preparation method of above-mentioned high covering power titanium dioxide, aluminum contained compound described in step b~e be containing
Meta-aluminic acid root or aluminum ions compound.
Further, in the preparation method of above-mentioned high covering power titanium dioxide, step d, alkalinity aluminum contained compound described in e is inclined
Sodium aluminate or potassium metaaluminate, preferably sodium metaaluminate.Acidity aluminum contained compound described in step b~d is aluminum sulfate, aluminium chloride or nitre
At least one of sour aluminium, preferably aluminum sulfate.
Further, in the preparation method of above-mentioned high covering power titanium dioxide, the adjusting pH contains calorize using acidity
Object or alkaline aluminum contained compound are closed, concentration is 100~110g/L.
The invention has the benefit that
The present invention provides a kind of preparation methods of high covering power titanium dioxide, by successively coating loose silicon oxide film, cause
Close pellumina, using weight sial coating during coating, so that coated product covering power has been increased to 99% or more.This hair
It is bright that pH is adjusted using acid aluminum contained compound or alkaline aluminum contained compound in the preparation, inorganic acid or alkali, the trip of generation are not added
It is few from acid, the wasting of resources is avoided, to more environment-friendly.The method of the present invention is easy to operate, the product strong covering power being prepared,
The dosage that titanium dioxide can be saved can be widely applied to the fields such as water paint, matt latex paint, water-based ink.
Detailed description of the invention
Fig. 1 is the TEM figure of 5 gained titanium dioxide product of the embodiment of the present invention.
Fig. 2 show the TEM figure of universal titanium dioxide R298.
Specific embodiment
The present invention provides a kind of preparation methods of high covering power titanium dioxide, comprising the following steps:
A, titanium dioxide first product is crushed, adds water that slurry is made, dispersing agent is added, adjusting slurry pH value is 9.0~11.0;
B, the obtained slurry of step a is heated to 40~60 DEG C, while silicon-containing compound and acid aluminum contained compound is added,
Keeping slurry pH value is 8.5~10.5, cures 30~60min;
C, acid aluminum contained compound is added in the slurry obtained to step b, adjusting slurry pH value is 4.0~6.5, curing 30
~60min;
D, acid aluminum contained compound and alkaline aluminum contained compound is added in cocurrent in the slurry obtained to step c, keeps slurry
PH value be 4.5~6.5, cure 30~60min;
E, the slurry pH value obtained by alkaline aluminum contained compound regulating step d is filtered, washing, is obtained after dry to 7.0~8.5
To high covering power titanium dioxide.
Wherein, titanium dioxide crude product described in step a refer to through sulfuric acid process or chloridising production it is not surface treated
Titanium dioxide.Preferably rutile titanium dioxide.Further, Ti content is 80~90% in the titanium dioxide.
Wherein, in order to improve the covering power of titanium dioxide, smashed partial size described in step a is 200~350nm.
Wherein, in order to preferably carry out coating, slurry concentration described in step a is 350g/L~450g/L.
Wherein, in order to keep the dispersion effect of slurry more preferable, dispersing agent described in step a is sodium metasilicate, calgon or list
At least one of isopropanolamine, additive amount are to make slurry viscosity 50cp~300cp.
In the present invention, if slurry concentration is too low, water content is too high in slurry, can reduce production efficiency, and slurry concentration is excessively high,
The uniform difficulty of coating increases, therefore the preferred 350g/L~450g/L of slurry concentration in step a.Dispersing agent additive amount is so that slurry is viscous
Degree is lower than 300cp;When dispersing agent additional amount is excessively high, slurry concentration is too low, can reduce production efficiency, waste of resource, preferably
, dispersing agent additive amount is so that slurry viscosity is 50cp~300cp.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, heating slurry temperature described in step b is preferably heated to
45 DEG C~55 DEG C.Temperature is too high, is unfavorable for coating operation.
Wherein, sparse porous silicon fiml, the present invention use weight sial coating, siliceous chemical combination described in step b in order to obtain
Object additive amount is 5.0~15.0% of titanium dioxide quality in slurry in terms of silica.What is be added when higher than existing coating contains
Silicon compound 3%.
Preferably, in the preparation method of above-mentioned high covering power titanium dioxide, the dosage of silicon-containing compound described in step b is with two
Silica meter is 6.0~10.0% of titanium dioxide quality in slurry.
Preferably, silicon-containing compound described in step b is sodium metasilicate or potassium silicate, and concentration is 280~300g/L.The present invention
By a large amount of repetition test, discovery, which improves sodium silicate silicate, can preferably be such that reaction carries out, but excessive concentration is in coating
It is easy to cause coating agent itself to be nucleated in the process, causes coating uneven.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, the additive amount of aluminum contained compound described in step b is with three
Al 2 O meter is 3.5~10.5% of titanium dioxide quality in slurry.Preferably 4.2~7.0%.
Specifically, the aluminum contained compound is to contain meta-aluminic acid root in the preparation method of above-mentioned high covering power titanium dioxide
Or aluminum ions compound.
Further, in the preparation method of above-mentioned high covering power titanium dioxide, the alkalinity aluminum contained compound is sodium metaaluminate
Or potassium metaaluminate, preferably sodium metaaluminate.The acidity aluminum contained compound is at least one in aluminum sulfate, aluminium chloride or aluminum nitrate
Kind, preferably aluminum sulfate.
Wherein, in the preparation method of above-mentioned high covering power titanium dioxide, the adjusting pH is using acid aluminum contained compound
Or alkaline aluminum contained compound.In order to not influence coating effect, the concentration of acid aluminum contained compound or alkaline aluminum contained compound is 100
The aqueous solution of~110g/L.It is higher that excessive concentration will cause local acid or alkali concentration, and capsule parts early period is caused to dissolve, itself
Nucleation, constituting on coating effect influences;Concentration is too low, introduces a large amount of water, reduces production efficiency.
Specifically, the key step of the preparation method of high covering power titanium dioxide of the present invention includes:
A, add water that slurry is made after crushed titanium dioxide first product, concentration is 350~450g/L, and dispersing agent is added and carries out
High speed dispersion to slurry viscosity is lower than 300cp, then adjusts the pH value of slurry to 9.0~10.0;Dispersing agent additive amount is so that slurry
Viscosity is 50cp~300cp;
B, sodium metasilicate is added to 45~55 DEG C in heating slurry, and adjusting slurry pH value is 8.5~11.0, and curing 30min~
60min;Wherein, sodium metasilicate additive amount is with the SiO in sodium metasilicate2Meter is TiO in slurry2The 5.0%~15.0% of quality;
C, aluminum contained compound is added into slurry after curing, and adjusting slurry pH value is 4.0~6.5, curing 30~
60min;
D, acid aluminum contained compound and alkaline aluminum contained compound is added in cocurrent, and keeps the PH of slurry in 4.5~6.5 ranges
It is interior, cure 30~60min;Wherein, aluminum contained compound additive amount is with the Al in aluminum contained compound2O3Meter is TiO in slurry2Quality
4.2%~7.0%;
E, slurry pH value is adjusted to 7.0~8.5 with alkaline aluminum contained compound, obtain high covering power after filtering, washing, drying
Titanium dioxide.
In the above method, step b, step c, the curing time of step d are unsuitable too long, and quickly coating is just easy to form loose
Porous coating, and the curing time too long economic value that can reduce coating.It is tested according to inventor, step b, when the curing of c, d
Between be 30~60min best.
The method of the present invention improves the covering power of titanium dioxide pigment.The coating agent dosage that the method for the present invention uses is big,
The covering power of titanium dioxide can be greatly improved, products obtained therefrom is used for indoor coating, the covering power of indoor coating can be improved.
The high covering power titanium dioxide of the method for the present invention preparation can be used to water paint after crushed, matt latex paint, water-based ink, make
The fields such as paper.
Explanation is further explained to a specific embodiment of the invention below in conjunction with embodiment, but is not indicated this
The protection scope of invention is limited in range described in embodiment.
Titanium dioxide first product in embodiment is the rutile titanium dioxide using Production By Sulfuric Acid Process, is purchased from Pan Gang group
Chongqing Tai Ye Co., Ltd.
Embodiment 1 prepares high covering power titanium dioxide using the method for the present invention
Specific step is as follows:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 350g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.0~10.0;
B, sodium metasilicate is added to 45 DEG C in heating slurry, and adjusting slurry pH value is 9.5 or so, with the SiO in sodium metasilicate2Meter
For TiO in slurry2The 6.0% of quality cures 30min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 4.5, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
4.2%, and keep the PH of slurry in 4.5~5.5 ranges, cure 60min;
E, slurry pH value is adjusted to 7.5 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Embodiment 2 prepares high covering power titanium dioxide using the method for the present invention
The present embodiment height covers method for producing rutile type titanium white powder and includes the following steps:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 350g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.0~10.0;
B, sodium metasilicate is added to 50 DEG C in heating slurry, and adjusting slurry pH value is 10.0, with the SiO in sodium metasilicate2It is calculated as starching
TiO in material2The 7.0% of quality cures 30min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 5.0, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
5.0%, and keep the PH of slurry in 4.5~5.5 ranges, cure 60min;
E, slurry pH value is adjusted to 8.0 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Embodiment 3 prepares high covering power titanium dioxide using the method for the present invention
The present embodiment height covers method for producing rutile type titanium white powder and includes the following steps:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 400g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, sodium metasilicate is added to 55 DEG C in heating slurry, and adjusting slurry pH value is 10.0, with the SiO in sodium metasilicate2It is calculated as starching
TiO in material2The 7.0% of quality cures 30min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 5.0, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
5.0%, and keep the PH of slurry in 4.5~5.0 ranges, cure 30min;
E, slurry pH value is adjusted to 8.0 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Embodiment 4 prepares high covering power titanium dioxide using the method for the present invention
The present embodiment height covers method for producing rutile type titanium white powder and includes the following steps:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 400g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, to 55 DEG C sodium metasilicate is added, with the SiO in sodium metasilicate in heating slurry2It is calculated as TiO in slurry2The 8.0% of quality,
Adjusting slurry pH value is 10.5, cures 30min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 5.5, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
5.6%, and keep the PH of slurry in 5.0~6.0 ranges, cure 30min;
E, slurry pH value is adjusted to 8.0 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Embodiment 5 prepares high covering power titanium dioxide using the method for the present invention
The present embodiment height covers method for producing rutile type titanium white powder and includes the following steps:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 400g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, sodium metasilicate is added to 55 DEG C in heating slurry, and adjusting slurry pH value is 10.5, with the SiO in sodium metasilicate2It is calculated as starching
TiO in material2The 9.0% of quality cures 40min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 5.5, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
6.3%, and keep the PH of slurry in 5.0~6.0 ranges, cure 30min;
E, slurry pH value is adjusted to 8.2 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Embodiment 6 prepares high covering power titanium dioxide using the method for the present invention
The present embodiment height covers method for producing rutile type titanium white powder and includes the following steps:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 450g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, to 55 DEG C sodium metasilicate is added, with the SiO in sodium metasilicate in heating slurry2It is calculated as TiO in slurry2Quality
10.0%, adjusting slurry pH value is 10.5, cures 50min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 6.0, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
7.0%, and keep the PH of slurry in 5.5~6.5 ranges, cure 30min;
E, slurry pH value is adjusted to 8.5 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Comparative example 7 does not use the method for the present invention to prepare titanium dioxide
Comparative example 7 is that weight sial coating (using general sial coating) is not used to prepare titanium dioxide, concrete operations step
It is rapid as follows:.
A, add water that slurry is made after crushed titanium dioxide first product, concentration 450g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, to 55 DEG C sodium metasilicate is added, with the SiO in sodium metasilicate in heating slurry2It is calculated as TiO in slurry2The 2.0% of quality,
Adjusting slurry pH value is 10.5, cures 50min;
C, acid aluminum sulfate solution is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH
Value is 6.0, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
1.5%, and keep the PH of slurry in 5.5~6.5 ranges, cure 30min;
E, slurry pH value is adjusted to 8.5 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Comparative example 8 does not use the method for the present invention to prepare titanium dioxide
Comparative example 8 be do not use low temperature coating (using high temperature) to prepare titanium dioxide, specific steps are as follows:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 450g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, to 85 DEG C sodium metasilicate is added, with the SiO in sodium metasilicate in heating slurry2It is calculated as TiO in slurry2The 2.5% of quality,
Adjusting slurry pH value is 10.5, cures 50min;
C, 60 DEG C are cooled to, to curing after acid aluminum sulfate solution be added in slurry reacted with remaining sodium silicate solution,
And adjusting slurry pH value is 5.0, cures 30min;
D, aluminum sulfate solution and sodium aluminate solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
2.0%, and keep the PH of slurry in 5.5~6.5 ranges, cure 60min;
E, slurry pH value is adjusted to 8.5 with sodium aluminate solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Comparative example 9 does not use the method for the present invention to prepare titanium dioxide
Comparative example 9 adjusts pH using inorganic acid and inorganic base, specific steps are as follows:
A, add water that slurry is made after crushed titanium dioxide first product, concentration 400g/L is added dispersing agent and carries out high speed
Slurry viscosity is dispersed to lower than 300cp, then adjusts the pH value of slurry to 9.5~10.5;
B, sodium metasilicate is added to 55 DEG C in heating slurry, and adjusting slurry pH value is 10.0, with the SiO in sodium metasilicate2It is calculated as starching
TiO in material2The 7.0% of quality cures 30min;
C, dilution heat of sulfuric acid is added into slurry after curing to react with remaining sodium silicate solution, and adjusts slurry pH value and is
5.0, cure 30min;
D, aluminum sulfate solution and sodium hydroxide solution is added in cocurrent, and additional amount is with Al2O3Meter is TiO in slurry2Quality
5.0%, and keep the PH of slurry in 4.5~5.0 ranges, cure 30min;
E, slurry pH value is adjusted to 8.0 with sodium hydroxide solution, filter, wash, obtain filter cake;
F, dry cake and product is crushed to obtain.
Separately below to Examples 1 to 6, the obtained titanium dioxide product of comparative example 7~9 and commercially available universal titanium white
Powder R298 (comparative example 10) carries out performance comparison.These titanium dioxides are configured to by formula and method as shown in table 1 below aqueous
Coating system.
1 experimental formula of table
Serial number | Title | Specification or model | Dosage (g) | Remarks |
1 | Desalted water | 130 | Technical grade | |
2 | Cellulose | 250HBR | 2.1 | Technical grade |
3 | PH adjusting agent | AMP~95 Tao Shi | 0.1g | Technical grade |
4 | Defoaming agent | BASF NXE | 1.0 | Technical grade |
5 | Wetting agent | BASF PE~100 | 1.5 | Technical grade |
6 | Dispersing agent | Ammonium salt 3000N | 1.5 | Technical grade |
7 | Titanium dioxide | Rutile-type | 100 | Technical grade |
The coating that embodiment and comparative example obtain is subjected to film and test in accordance with the following methods:
1) black and white lattice paper jam is placed on the vacuum chuck of automatic spray device;
2) 100 μm of wet film makers are placed on black and white lattice paper jam, and be fixed on automatic spray device.
3) it takes suitable aqueous color paste slurry to be uniformly placed on black and white lattice paper jam top of supply line, starts automatic film applicator, system
Thickness is identical and uniform paint film.
4) paint film made is horizontally arranged, is placed in air for 24 hours, after surface of the paint film finishes, test its covering power.
5) the opacity N on black-film is tested respectively with whiteness instrument1With the opacity N in white tiles2。
6) the opacity N of black-film is used1Divided by the opacity N of white tiles2, obtain contrast ratio η (i.e. covering power).Each sample
8 groups of data are tested, respective contrast ratio is calculated, is then averaged, obtain result as shown in table 2 below.
Wherein, covering power
The detection case of 2 coated product of table covering power in aqueous color paste system
From the applied performance analysis of above each example, in the application field aqueous coating system of titanium dioxide of the present invention, this hair
Compared with the titanium dioxide of conventional method, covering power and whiteness performance are greatly improved the titanium dioxide of bright method production, and use
Sulfate replaces diluted acid and diluted alkaline, further decreases production cost and environmentally friendly cost.
2. transmission electron microscope detects
5 gained titanium dioxide product of the embodiment of the present invention is detected through transmission electron microscope, gained TEM figure is as shown in Figure 1.And figure
The 2 existing universal products are compared, and the low temperature quick alkaline cladding silica that the method for the present invention uses is capable of forming loose porous dioxy
SiClx film is more advantageous to covering power of the product in water-based system.
According to the experimental results, the present invention provides a kind of preparation method of high covering power titanium dioxide, the titanium dioxides of preparation
Covering power can reach 99.5% or more, this improves one percentage point than the covering power of existing titanium dioxide 98.5% or so,
In titanium dioxide preparation field, the covering power for improving a point is extremely not easy, and the present invention achieves significant progress, the titanium of preparation
White powder strong covering power has widened the application field of titanium dioxide.
Claims (10)
1. the preparation method of high covering power titanium dioxide, which comprises the following steps:
A, titanium dioxide first product is crushed, adds water that slurry is made, dispersing agent is added, adjusting slurry pH value is 9.0~11.0;
B, the obtained slurry of step a is heated to 40~60 DEG C, while silicon-containing compound and acid aluminum contained compound is added, kept
Slurry pH value is 8.5~10.5, cures 30~60min;
C, acid aluminum contained compound is added in the slurry obtained to step b, adjusting slurry pH value is 4.0~6.5, curing 30~
60min;
D, acid aluminum contained compound and alkaline aluminum contained compound is added in cocurrent in the slurry obtained to step c, keeps the pH of slurry
Value is 4.5~6.5, cures 30~60min;
E, the slurry pH value obtained by alkaline aluminum contained compound regulating step d filters, washing obtains height after dry to 7.0~8.5
Covering power titanium dioxide.
2. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: after being crushed described in step a
Partial size be 200~350nm.
3. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: slurry described in step a
Concentration is 350g/L~450g/L.
4. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: dispersing agent described in step a
For at least one of sodium metasilicate, calgon or monoisopropanolamine, additive amount is to make slurry viscosity 50cp~300cp.
5. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: siliceous described in step b
Compound additive amount is 5.0~15.0% of titanium dioxide quality in slurry in terms of silica.
6. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: siliceous described in step b
Compound is sodium metasilicate or potassium silicate, and concentration is 280~300g/L.
7. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: contain aluminium described in step b
The additive amount of compound is 3.5~10.5% of titanium dioxide quality in slurry in terms of aluminum oxide.
8. the preparation method of high covering power titanium dioxide according to claim 1, it is characterised in that: contain aluminium described in step b~e
Compound is to contain meta-aluminic acid root or aluminum ions compound.
9. the preparation method of high covering power titanium dioxide according to claim 8, it is characterised in that: step d, alkalinity described in e
Aluminum contained compound is sodium metaaluminate or potassium metaaluminate, preferably sodium metaaluminate.
10. the preparation method of high covering power titanium dioxide according to claim 8, it is characterised in that: acid described in step b~d
Property aluminum contained compound be at least one of aluminum sulfate, aluminium chloride or aluminum nitrate, preferably aluminum sulfate.
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CN108997791A (en) * | 2018-09-05 | 2018-12-14 | 襄阳龙蟒钛业有限公司 | A kind of high glaze titanium dioxide |
CN110988037A (en) * | 2019-11-20 | 2020-04-10 | 攀钢集团重庆钛业有限公司 | Method for detecting dispersion state of titanium dioxide |
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CN114539811A (en) * | 2022-03-01 | 2022-05-27 | 昆明冶金研究院有限公司 | High-covering-performance easily-dispersible silica fume and preparation method thereof |
CN116023806A (en) * | 2022-09-22 | 2023-04-28 | 攀枝花东方钛业有限公司 | Titanium dioxide for environment-friendly paint and preparation method thereof |
CN115651426A (en) * | 2022-10-24 | 2023-01-31 | 攀钢集团研究院有限公司 | Method for preparing titanium white special for printing ink by using hydrochloric acid as chlorination byproduct |
CN116285425A (en) * | 2022-12-15 | 2023-06-23 | 宜宾天原海丰和泰有限公司 | Titanium dioxide silicon-aluminum coating method |
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