CN104194410A - Preparation method of titanium dioxide pigment - Google Patents
Preparation method of titanium dioxide pigment Download PDFInfo
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- CN104194410A CN104194410A CN201410404059.7A CN201410404059A CN104194410A CN 104194410 A CN104194410 A CN 104194410A CN 201410404059 A CN201410404059 A CN 201410404059A CN 104194410 A CN104194410 A CN 104194410A
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Abstract
The invention belongs to the field of titanium dioxide production, particularly relates to a preparation method of a titanium dioxide pigment, and aims at solving the technical problem of providing a preparation method of a titanium dioxide pigment which is high in weather fastness and relatively friendly to environment. In order to solve the technical problem, according to the technical scheme, the preparation method comprises the following steps: firstly, carrying out silica coating on a silica primary product; then carrying out aluminum phosphate coating; and finally, carrying out alkaline coating on aluminum oxide to form a boehmite type aluminum oxide coating. According to the invention, coating is carried out by adopting the method, so that the light resistance and the weather fastness of the product are improved, and meanwhile, the dispersing performance of the product is also improved. According to the method, the addition of the phosphoric acid is relatively low, the generated free phosphoric acid is little, so resource waste is avoided, and the method is relatively friendly to environment.
Description
Technical field
The invention belongs to titanium dioxide production field, be specifically related to a kind of preparation method of TiO 2 pigment.
Background technology
Titanium dioxide (TiO
2) be a kind of white pigment, be often applied to numerous areas, in coating, plastics, paper, veneer sheet or other coating systems.At TiO
2in surface-treated process, add under given conditions some chemical and can significantly increase pigment needed performance in product application.As in opacifying power, dispersiveness and light stability.
Not surface treated titanium dioxide weather resistance is poor, if in surface-treated process, add under given conditions the weather resistance that some chemical can obviously strengthen pigment, modal is some compounds of cerium, zirconium, silicon, phosphorus, aluminium, and titanium dioxide manufacturers solves this problem by various effort by the surface treatment of pigment both at home and abroad.
US Patent No. 5785748 discloses a kind of technique for the manufacture of TiO 2 pigment, it is the solution at heating in the situation that and aluminum compound reaction generation clear by strong phosphoric acid, then the solution after dilution is joined in titanium dioxide slurry, and add a kind of basic cpd to make slurry pH at least reach 3.5; And before slurry drying, add a kind of compound as oxygenant to be coated to improve the photostabilization of TiO 2 pigment as saltpetre, Potassium Iodate or copper sulfate etc.This method is due to significantly excessive guarantee solution transparent of phosphoric acid in the time that phosphoric acid salt is prepared, and a large amount of free phosphoric acid can only neutralize with alkali, has caused the waste of resource.
US Patent No. 4461810 discloses a kind of sunproof method of raising titanium dioxide, adds a kind of cerium salt to guarantee the photostabilization of titanium dioxide in the coating agent of titanium dioxide.But cerium salt may make the form and aspect of titanium dioxide partially yellow, and can significantly increase production cost.
US Patent No. 061013A2 discloses a kind of technique of prepared layer platen special titanium pigment, this invention is water-based titania slurry, do not need to add dispersion agent and only carry out coating by adjusting pH value, coating layer is the coated aluminum phosphate of the first layer, second layer coated aluminum oxide.This inventive method requires the amount of coated phosphoric acid larger, and approximately 2.2～5.0%, easily cause having a large amount of free phosphoric acid in filtrate, cause environmental pollution, and its slurry do not add dispersion agent to be only adapted to chlorination process first product, its product does not reach the requirement of weathering resistance.
Chinese patent CN101857736A discloses a kind of sunproof method that improves titanium dioxide by zirconium, phosphorus, aluminium coating.But zirconium is a kind of relatively costly raw material, in actual production, can increase production cost, and it is limited to improve photostabilization effect.
Chinese patent CN1850915A discloses a kind of method of utilizing sial coating to improve the weathering resistance of titanium dioxide, but this invention requires the covering amount of silicon oxide and aluminum oxide can not be lower than 3.5%, and coating temperature, lower than 85 DEG C, is unfavorable for forming fine and close silicon oxide film.
Chinese patent CN103709792A utilize the coated water glass of following current and and flow aluminum phosphate and be coated, and covering amount is larger, but the method following current coated silica is fine and close not, cause product weathering resistance not good enough, and phosphoric acid amount is more, cause aluminum phosphate self film forming, reduce weathering resistance.And there is a large amount of free phosphoric acid in filtrate in excessive easily causing of phosphoric acid, causes environmental pollution.
Therefore, those skilled in the art need that a kind of weathering resistance is high, preparation method to the more friendly TiO 2 pigment of environment.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of weathering resistance is high, preparation method to the more friendly TiO 2 pigment of environment.For solving the problems of the technologies described above, the technical solution adopted in the present invention comprises the following steps:
A, add water and make slurry after titanium dioxide first product is pulverized, add dispersion agent, then to regulate slurry pH value be 9.0～11.0;
B, heating slurry to 80 DEG C～100 DEG C, add water glass, and regulating slurry pH value is 8.0～10.0, slaking;
C, the slurry after slaking is cooled to 50 DEG C～70 DEG C, adds phosphate compounds, and stream adds aluminum contained compound so that generate aluminum phosphate, that controls phosphate compounds and aluminum contained compound adds speed so that slurry pH value is 5.0～9.0, slaking;
D, in slurry, add aluminum contained compound to react with remaining phosphate compounds, and stream to regulate slurry pH value be 9.5～10.5, slaking;
E, adjusting slurry pH value to 7.0～8.0, filter, wash, be dried, pulverize and to obtain product;
Wherein, step b mesosilicic acid sodium addition, in silicon-dioxide, is 1.0%～5.0% of titanium dioxide quality in slurry; Preferably, water glass addition, in silicon-dioxide, is 1.5%～3.5% of titanium dioxide quality in slurry; In step c, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～2% of quality; Preferably, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～1.5% of quality; In steps d, aluminum contained compound addition is with the Al in aluminum contained compound
2o
3meter is TiO in slurry
22.0%～4.0% of quality.
Described in technical solution of the present invention step a, titanium dioxide first product is rutile titanium dioxide first product.
In technique scheme, slurry concentration is too low, and in slurry, water content is too high, can reduce production efficiency, slurry concentration is too high, and the inhomogeneity difficulty of coating strengthens, therefore the preferred 250g/L～350g/L of slurry concentration in step a, dispersion agent addition so that slurry viscosity lower than 300cp; Too high when dispersion agent add-on, slurry concentration is too low, can reduce production efficiency, waste resource, and preferred, dispersion agent addition is so that slurry viscosity is 50cp～300cp.
In technique scheme, dispersion agent described in step a is preferably at least one in water glass, Sodium hexametaphosphate 99, monoisopropanolamine.
If temperature is too low, silicon-dioxide coating compactness is not good enough, and excess Temperature is unfavorable for coating operation, preferred, step b heating slurry temperature to 80 DEG C～95 DEG C; More excellent, heating slurry temperature to 85 DEG C～90 DEG C.
In step b, regulate pH value can adopt the mode of following current to add, the mode that also can adopt and flow adds, acid adding mode on silicon-dioxide coating without impact.
At least one in technique scheme in an alkali metal salt of phosphate compounds preferably phosphoric acid, Sodium hexametaphosphate 99, ammonium phosphate, sodium hydrogen phosphate, phosphoric acid.
Phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～2% of quality, if exceed 2.0%, can cause particle coacervation, reduces the dispersing property of pigment and the opacity of coating and gloss.Preferably, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～1.5% of quality.
Concrete, the aluminum contained compound in technique scheme is to contain meta-aluminic acid root or aluminum ions compound, preferably at least one in sodium metaaluminate, potassium metaaluminate, Tai-Ace S 150, aluminum chloride, aluminum nitrate.
Concrete, the curing time of step b, step c, steps d, while being 30min～60min, is wrapped up best results.
Adjusting slurry pH value described in technique scheme is according to target pH value, adds mineral acid or alkali; Described mineral acid is preferably at least one in sulfuric acid, hydrochloric acid, nitric acid; Described alkali is at least one in sodium hydroxide, potassium hydroxide.Further, described in add mineral acid or alkali adds taking concentration as 10wt%～30wt% aqueous solution, excessive concentration can cause local acid or alkali concn higher, cause early stage coating to be partly dissolved, the densification of coating is formed to impact; Concentration is too low, introduces a large amount of water, reduces production efficiency.
Titanium dioxide first product described in the present invention refers to the not surface treated titanium dioxide through sulfuric acid process or chlorination process production.
Process through aforesaid method the high weathering resistance titanium dioxide pigment obtaining and can be used for after crushed the fields such as water-borne coatings, plastics, ink and papermaking.
Beneficial effect of the present invention is as follows:
1, the inventive method coated close silicon oxide, aluminum phosphate, aluminum oxide successively, photostabilization and the weathering resistance of products obtained therefrom are all significantly increased, and especially, adopt alkaline coated aluminum oxide can form boehmite-type aluminum oxide, are more conducive to strengthen the dispersing property of product.
2, the inventive method phosphoric acid add-on is few, and the free phosphoric acid of generation is few, has avoided the wasting of resources, and more excellent good to environment.
Brief description of the drawings
Fig. 1 is the TEM figure according to CN103709792A embodiment 1 method gained titanium dioxide product;
Fig. 2 is the TEM figure of the embodiment of the present invention 2 gained titanium dioxide products.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The technical solution adopted in the present invention comprises the following steps:
A, titanium dioxide first product is added water after crushed and makes slurry, concentration is 250～350g/L, add dispersion agent carry out high speed dispersion to slurry viscosity lower than 300cp, then regulate pH value to 9.0～11.0 of slurry; Preferably, dispersion agent addition is so that slurry viscosity is 50cp～300cp;
B, heating slurry to 80～100 DEG C, add water glass, and regulating slurry pH value is 8.0～10.0, slaking 30min～60min;
C, the slurry after slaking is cooled to 50 DEG C～70 DEG C, add phosphate compounds, and stream adds aluminum contained compound so that generate aluminum phosphate, that controls phosphate compounds and aluminum contained compound adds speed so that slurry pH value is 5.0～9.0, slaking 30min～60min;
D, in slurry, add aluminum contained compound to react with remaining phosphate compounds, and stream to regulate slurry pH value be 9.5～10.5, slaking 30min～60min;
It is 7.0～8.0 that e, acid adding regulate the pH value of slurry, filters, washes, is dried, pulverizes and to obtain product;
Wherein, step b mesosilicic acid sodium addition, in silicon-dioxide, is 1.0%～5.0% of titanium dioxide quality in slurry; Preferably, water glass addition, in silicon-dioxide, is 1.5%～3.5% of titanium dioxide quality in slurry; In step c, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～2% of quality; Preferably, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～1.5% of quality; In steps d, aluminum contained compound addition is with the Al in aluminum contained compound
2o
3meter is TiO in slurry
22.0%～4.0% of quality.
Wherein, the dispersion agent in step a can be selected from least one in water glass, Sodium hexametaphosphate 99 and monoisopropanolamine.
Wherein, the phosphate compounds in steps d can be selected from least one in the phosphate compounds such as an alkali metal salt of phosphoric acid, Sodium hexametaphosphate 99, ammonium phosphate, phosphoric acid.
Concrete, above-mentioned aluminum contained compound is to contain meta-aluminic acid root or aluminum ions compound, preferably at least one in sodium metaaluminate, potassium metaaluminate, Tai-Ace S 150, aluminum chloride, aluminum nitrate.
The too short formation that is unfavorable for dense film of curing time of step b, step c, steps d, curing time proper extension is conducive to the formation of dense film, but the long economic worth that can reduce coating of curing time.According to contriver's experiment, the curing time of step b, c, d is 30min～60min the best.
Adjusting slurry pH value described in technique scheme, for according to demand, adds mineral acid or alkali; Described mineral acid is preferably at least one in sulfuric acid, hydrochloric acid, nitric acid; Described alkali is at least one in sodium hydroxide, potassium hydroxide.Further, described in add mineral acid or alkali adds taking concentration as 10wt%～30wt% aqueous solution, excessive concentration can cause local acid or alkali concn higher, cause early stage coating to be partly dissolved, the densification of coating is formed to impact; Concentration is too low, introduces a large amount of water, reduces production efficiency.
Process through aforesaid method the high weathering resistance titanium dioxide pigment obtaining and can be used for after crushed the fields such as water-borne coatings, plastics, ink and papermaking.
The inventive method has been improved the light stability of TiO 2 pigment.The phosphoric acid salt that the inventive method is introduced can reduce the photocatalytic effect of titanium dioxide, and products obtained therefrom, for laminated paper, can improve the light stability of laminated paper products.
Below in conjunction with embodiment, the present invention is further described.
In order better to understand the impact of different titanium dioxide effects on surface processing, embodiment selects three groups of titanium dioxide:
1) the titanium dioxide first product in embodiment 1-3 adopts the rutile titanium dioxide of Production By Sulfuric Acid Process, purchased from Pangang Group Chongqing Titanium Co., Ltd, and salt treatment agent: zinc salt and sylvite;
2) the titanium dioxide first product in embodiment 4-6 adopts the rutile titanium dioxide of Production By Sulfuric Acid Process, purchased from east Tai Ye company limited of Pan Gang group, salt treatment agent: aluminium salt;
3) the titanium dioxide first product in embodiment 7-9 adopts the rutile titanium dioxide that chlorination process is produced, purchased from Jinzhou Titanium Industry Co., Ltd..
Embodiment 1
A, get 250g titanium dioxide first product, after pulverizing, be made into deionized water the slurry that concentration is 250g/L, adding monoisopropanolamine to be dispersed to slurry viscosity is 220cp, and regulates the pH value to 9.0 of slurry with sodium hydroxide solution;
B, heating slurry to 85 DEG C, add water glass, and described water glass addition is with SiO in water glass
2meter is TiO in slurry
21.5% of quality, and flow acid adding to control the pH value of slurry as 9.5～10.0, slaking 30min;
C, slurry temperature are down to 50 DEG C, add sodium hydrogen phosphate, and stream adds Tai-Ace S 150 so that generate aluminum phosphate, and that controls sodium hydrogen phosphate and Tai-Ace S 150 adds speed so that slurry pH value is 5.0～9.0; Wherein, sodium hydrogen phosphate addition is with P in sodium hydrogen phosphate
2o
5count TiO in slurry
21.5% of quality, slaking 30min;
D, add the Tai-Ace S 150 sodium hydrogen phosphate complete with unreacted to continue to react, and stream adds alkali taking the pH value that maintains slurry as 9.5～10.5, wherein, Tai-Ace S 150 addition is with Al in Tai-Ace S 150
2o
3count TiO in slurry
24.0% of quality, slaking 60min;
E, adjustment slurry pH value to 8.0, filter, wash, and obtains filter cake;
F, dry cake are also pulverized to obtain product.
Embodiment 2
A, get 300g titanium dioxide first product, after pulverizing, be made into deionized water the slurry that concentration is 270g/L, adding monoisopropanolamine to be dispersed to slurry viscosity is 150cp, and adds alkali and regulate the pH value to 10.0 of slurry;
B, heating slurry to 87 DEG C, add water glass, and described water glass addition is with SiO in water glass
2meter is TiO in slurry
22.5% of quality, and flow acid adding to control the pH value of slurry as 9.5～10.0, slaking 60min;
C, slurry temperature are down to 60 DEG C, add phosphoric acid, and stream adds sodium metaaluminate so that generate aluminum phosphate, and that controls phosphoric acid and sodium metaaluminate adds speed so that slurry pH value is 5.0～9.0; Wherein, phosphoric acid addition is with P in phosphoric acid
2o
5count TiO in slurry
21.0% of quality, slaking 60min;
D, add the sodium metaaluminate phosphoric acid complete with unreacted to continue to react, and flow acid adding with the pH value that maintains slurry between 9.5～10.5, wherein, sodium metaaluminate addition is with Al in sodium metaaluminate
2o
3count TiO in slurry
23.0% of quality, slaking 60min;
The pH value to 7.5 of e, adjustment slurry, filters, washes, and obtains filter cake;
F, dry cake are also pulverized to obtain product.
Embodiment 3
A, get 350g titanium dioxide first product, after pulverizing, be made into deionized water the slurry that concentration is 280g/L, adding Sodium hexametaphosphate 99 to be dispersed to slurry viscosity is 240cp, and adds alkali and regulate the pH value to 11.0 of slurry;
B, heating slurry to 90 DEG C, add water glass, and described water glass addition is with SiO in water glass
2count TiO in slurry
23.5% of quality, and flow acid adding to control the pH value of slurry as 9.5～10.0, slaking 30min;
C, slurry temperature are down to 70 DEG C, add Sodium hexametaphosphate 99, and stream adds sodium metaaluminate so that generate aluminum phosphate, and that controls Sodium hexametaphosphate 99 and sodium metaaluminate adds speed so that slurry pH value is 5.0～9.0; Wherein, Sodium hexametaphosphate 99 addition is with the P of Sodium hexametaphosphate 99
2o
5count TiO in slurry
20.5% of quality, slaking 30min;
D, add the sodium metaaluminate Sodium hexametaphosphate 99 complete with unreacted to continue react, and flow acid adding taking control pH value as 9.5～10.5, wherein, sodium metaaluminate addition is with Al in sodium metaaluminate
2o
3count TiO in slurry
22.0% of quality, slaking 60min;
The pH value to 7.0 of e, adjustment slurry, filters, washes, and obtains filter cake;
F, dry cake are also pulverized to obtain product.
Embodiment 4
According to embodiment 1 method preparation.
Embodiment 5
According to embodiment 2 method preparations.
Embodiment 6
According to embodiment 3 method preparations.
Embodiment 7
According to embodiment 1 method preparation.
Embodiment 8
According to embodiment 2 method preparations.
Embodiment 9
According to embodiment 3 method preparations.
Below the titanium dioxide product respectively above-described embodiment 1～9 being obtained and the light stability of titanium dioxide of the prior art, acid-soluble rate are measured.
A, light stability are measured
Detection method: the product that embodiment 1～9 is obtained, sneak in proportion respectively in water miscible terpolycyantoamino-formaldehyde resin, then coat on model, with the weather-proof instrument irradiation of Q-SUN1000 type, after pre-irradiation, use the each survey of whiteness instrument L, an a, b value, aberration Δ E after pre-irradiation calculates by following formula, and Δ E is larger represents that the photostabilization of model is poorer.
Wherein, the brightness of L-pre-irradiation, the red green phase of a-pre-irradiation, the champac form and aspect of b-pre-irradiation, the postradiation brightness of L*-, the postradiation red green phase of a*-, the postradiation champac form and aspect of b*-.
The result that detects embodiment 1～9 pigment and comparative example gained is as shown in table 1.
Table 1
Remarks: comparative example 1 is external laminated paper special product, comparative example 2 is domestic papermaking special product.
From table 1, data can be found out, above-described embodiment gained TiO 2 pigment has higher photostabilization, illustrate that fine and close water glass film can improve the sun-proof performance of pigment preferably in conjunction with fine and close aluminum phosphate film.
B, acid-soluble rate detect
In the field such as coating, plastics, the weathering resistance of TiO 2 pigment is had relatively high expectations, acid-soluble rate detects can rapid detection pigment weathering resistance.TiO
2surface coated Si O
2densification and integrated degree can by detect the acid-soluble of sample evaluate, loose SiO
2deposition can not be coated TiO completely
2surface, cause acid-soluble rate higher; The SiO of even compact
2coating layer will obtain lower acid-soluble rate, and the weathering resistance of the lower expression product of acid-soluble rate is better.
Coating TiO
2the acid-soluble rate of pigment detects, by the TiO of 0.2000g coating
2pigment adds in 98% vitriol oil 10ml, is heated to 175 DEG C and dissolves 1h, cooling, after dilution, filters, and gets filtrate and detects absorbancy, calculates soluble T iO according to typical curve
2concentration.Acid-soluble rate is the TiO of solubility
2percentage composition, available soluble TiO
2concentration calculates by formula.Embodiment 1-9 gained titanium dioxide product and comparative example 1, comparative example 2 are carried out to acid-soluble rate test, and acid-soluble rate data are in table 2.
Table 2
Remarks: comparative example 1 is external laminated paper special product, comparative example 2 is domestic papermaking special product.
As can be seen from Table 2, the photostabilization of the inventive method products obtained therefrom and weathering resistance have all had significant lifting.
C, transmission electron microscope detect
Detect through transmission electron microscope according to CN103709792A embodiment 1 method gained titanium dioxide product, gained TEM schemes as shown in Figure 1.
The embodiment of the present invention 2 gained titanium dioxide products are detected through transmission electron microscope, and gained TEM schemes as shown in Figure 2.
The alkaline coated aluminum oxide that the inventive method adopts can form boehmite-type aluminum oxide, is more conducive to the dispersion of product in all kinds of systems.And paired observation Fig. 1 and Fig. 2 known, in Fig. 1, have part film forming, but film forming is inhomogeneous, the film forming in Fig. 2 is more even, fine and close.The inventive method products obtained therefrom compactness and weathering resistance are better.
Claims (10)
1. the preparation method of TiO 2 pigment, is characterized in that, comprises the following steps:
A, add water and make slurry after titanium dioxide first product is pulverized, add dispersion agent, then to regulate slurry pH value be 9.0～11.0;
B, heating slurry to 80 DEG C～100 DEG C, add water glass, and regulating slurry pH value is 8.0～10.0, slaking;
C, the slurry after slaking is cooled to 50 DEG C～70 DEG C, adds phosphate compounds, and stream adds aluminum contained compound so that generate aluminum phosphate, that controls phosphate compounds and aluminum contained compound adds speed so that slurry pH value is 5.0～9.0, slaking;
D, in slurry, add aluminum contained compound to react with remaining phosphate compounds, and stream to regulate slurry pH value be 9.5～10.5, slaking;
E, adjusting slurry pH value to 7.0～8.0, filter, wash, be dried, pulverize and to obtain product;
Wherein, step b mesosilicic acid sodium addition, in silicon-dioxide, is 1.0%～5.0% of titanium dioxide quality in slurry; Preferably, water glass addition, in silicon-dioxide, is 1.5%～3.5% of titanium dioxide quality in slurry; In step c, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～2% of quality; Preferably, phosphate compounds addition is with P
2o
5count TiO in slurry
20.5%～1.5% of quality; In steps d, aluminum contained compound addition is with the Al in aluminum contained compound
2o
3meter is TiO in slurry
22.0%～4.0% of quality.
2. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: in step a, slurry concentration is 250g/L～350g/L, dispersion agent addition so that slurry viscosity lower than 300cp; Preferably, dispersion agent addition is so that slurry viscosity is 50cp～300cp.
3. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: in step a, dispersion agent used is at least one in water glass, Sodium hexametaphosphate 99, monoisopropanolamine.
4. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: step b heating slurry temperature to 80 DEG C～95 DEG C; More excellent, heating slurry temperature to 85 DEG C～90 DEG C.
5. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: step b adjusting slurry pH value employing following current or the also mode of stream add.
6. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: described phosphate compounds is at least one in an alkali metal salt of phosphoric acid, Sodium hexametaphosphate 99, ammonium phosphate, sodium hydrogen phosphate, phosphoric acid.
7. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: described in step c, steps d, aluminum contained compound is to contain meta-aluminic acid root or aluminum ions compound; Preferably at least one in sodium metaaluminate, potassium metaaluminate, Tai-Ace S 150, aluminum chloride, aluminum nitrate.
8. the preparation method of TiO 2 pigment according to claim 1, is characterized in that: step b, step c, steps d curing time are 30min～60min.
9. according to the preparation method of the TiO 2 pigment described in claim 1～8 any one, it is characterized in that: described adjusting slurry pH value is for adding mineral acid or alkali; Described mineral acid is preferably at least one in sulfuric acid, hydrochloric acid, nitric acid; Described alkali is at least one in sodium hydroxide, potassium hydroxide; Further, described in, adding mineral acid or alkali adds taking concentration as 10wt%～30wt% aqueous solution.
10. according to the preparation method of the TiO 2 pigment described in claim 1～9 any one, it is characterized in that: the first product of titanium dioxide described in step a is rutile titanium dioxide first product.
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