CN107828248B - Titanium dioxide for plastic color master batch - Google Patents

Titanium dioxide for plastic color master batch Download PDF

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CN107828248B
CN107828248B CN201711103903.2A CN201711103903A CN107828248B CN 107828248 B CN107828248 B CN 107828248B CN 201711103903 A CN201711103903 A CN 201711103903A CN 107828248 B CN107828248 B CN 107828248B
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titanium dioxide
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metatitanic acid
equal
acid slurry
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CN107828248A (en
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朱永昌
钟振华
罗勇
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Guangxi Shun Feng Titanium Industry Co Ltd
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Guangxi Shun Feng Titanium Industry Co Ltd
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Abstract

The invention provides titanium dioxide and TiO for plastic color master batch2The content of (a) is 95.5-98.5 wt%, wherein, the rutile type TiO2The content of (A) is more than or equal to 98.7 wt%; particle diameter D500.23 to 0.27 μm, particle diameter D99Less than or equal to 0.5 mu m. The titanium dioxide for the plastic color master batch provided by the invention has high whiteness, dispersibility, covering power and oil absorption, and can meet the requirements of the plastic industry on the performance of the titanium dioxide. The performance index analysis of the titanium dioxide for the plastic color master batch shows that the color phase L value of the titanium dioxide for the plastic color master batch is more than or equal to 98.5 percent, the b value is less than or equal to 1.4, the a value is less than or equal to 0.3, the dispersity is more than or equal to 7.0, the decolorization rate is 110 percent, and the oil absorption is (11-13) g/100 g.

Description

Titanium dioxide for plastic color master batch
Technical Field
The invention relates to the technical field of chemical raw materials, in particular to titanium dioxide for plastic color master batches.
Background
Titanium dioxide (TiO) with titanium dioxide name2) Mainly has two crystal forms of rutile type and anatase type. Titanium dioxide has the advantages of excellent whiteness, tinting strength, covering power and the like, has the highest refractive index in all white pigments, is considered to be the best white pigment, and is widely applied to the industries of coatings, plastics, printing, rubber and the like.
The titanium dioxide is applied to the plastic color master batch, and can improve the heat resistance, light resistance and weather resistance of plastic products besides utilizing the high covering power, high tinting strength and other pigment properties of the titanium dioxide. The titanium dioxide powder of the color master batch is positioned in the core layer of the color master batch, so the requirements on whiteness, dispersibility, covering power, oil absorption and the like are higher, and the titanium dioxide powder in the prior art is difficult to meet the requirements, such as the hue b value of about 1.6-1.8, the dispersibility of about 6.5 and the oil absorption of about (16-20) g/100 g. Therefore, the titanium dioxide product with higher whiteness, better dispersibility, better covering power and better oil absorption is a technical problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to provide the titanium dioxide for the plastic color master batch, which has high whiteness, good dispersibility, good covering power and good oil absorption and can meet the requirements of the plastic industry on the performance of the titanium dioxide.
The invention provides titanium dioxide and TiO for plastic color master batch2The content of (a) is 95.5-98.5 wt%, wherein, the rutile type TiO2The content of (A) is more than or equal to 98.7 wt%; particle diameter D500.23 to 0.27 μm, particle diameter D99≤0.5μm。
Preferably, Al is further included2O3Said Al2O3The content of (B) is 0.8-1.2 wt%.
Preferably, the paint also comprises trimethylchlorosilane, and the content of the trimethylchlorosilane is 0.7-1.0 wt%.
Preferably, it also comprises Fe2O3Said Fe2O3The content of (B) is less than or equal to 0.005 wt%.
Preferably, the content of 45 μm screen residue is 0.01 wt% or less.
Preferably, the specific surface area is 13-15 m2/g。
Preferably, the volatile matter after drying for 2 hours at 105 ℃ is less than or equal to 0.2 wt%.
Preferably, the drying is carried out for 2h at 105 ℃, and the ignition loss after 1h ignition is less than or equal to 0.3 wt% at 900 ℃.
The invention provides titanium dioxide and TiO for plastic color master batch2The content of (a) is 95.5-98.5 wt%, wherein, the rutile type TiO2The content of (A) is more than or equal to 98.7 wt%; particle diameter D500.23 to 0.27 μm, particle diameter D99Less than or equal to 0.5 mu m. The titanium dioxide for the plastic color master batch provided by the invention has high whiteness, dispersibility, covering power and oil absorption, and can meet the requirements of the plastic industry on the performance of the titanium dioxide. The performance index analysis of the titanium dioxide for the plastic color master batch shows that the color phase L value of the titanium dioxide for the plastic color master batch is more than or equal to 98.5 percent, the b value is less than or equal to 1.4, the a value is less than or equal to 0.3, the dispersity is more than or equal to 7.0, the decolorization rate is 110 percent (taking the decolorization rate of the titanium dioxide in the prior art as a reference), and the oil absorption is (11-13) g/100 g.
Detailed Description
The invention provides titanium dioxide and TiO for plastic color master batch2The content of (a) is 95.5-98.5 wt%, wherein, the rutile type TiO2In an amount ofMore than or equal to 98.7 wt%; particle diameter D500.23 to 0.27 μm, particle diameter D99≤0.5μm。
In the invention, TiO in the titanium dioxide for the plastic color master batch2The content of (B) is 95.5 to 98.5 wt%, preferably 96 to 98 wt%, more preferably 96.5 to 97.5 wt%, most preferably 97 wt%.
In the present invention, the TiO is2Including rutile TiO2The rutile type TiO2The content of (B) is not less than 98.7 wt%, preferably not less than 99.3 wt%, more preferably not less than 99.9 wt%.
In the invention, the particle size D of the titanium dioxide for the plastic color master batch500.23 to 0.27 μm, preferably 0.24 to 0.26 μm; particle diameter D99Less than or equal to 0.5 μm, preferably less than or equal to 0.4 μm, more preferably less than or equal to 0.3. mu.m.
In the invention, the titanium dioxide for the plastic color master batch preferably also comprises Al2O3Said Al2O3The content of (B) is preferably 0.8 to 1.2 wt%, more preferably 0.9 to 1.1 wt%, most preferably 1.0 wt%.
In the invention, the titanium dioxide for the plastic color master batch preferably further comprises trimethylchlorosilane, and the content of the trimethylchlorosilane is preferably 0.7-1.0 wt%, and more preferably 0.8-0.9 wt%.
In the invention, the preferable titanium dioxide for the plastic color master batch also comprises Fe2O3Said Fe2O3The content of (B) is preferably 0.005% by weight or less, more preferably 0.004% by weight or less, most preferably 0.003% by weight or less.
In the invention, the content of the titanium dioxide 45 μm screen residue for the plastic color master batch is preferably less than or equal to 0.01 wt%, more preferably less than or equal to 0.008 wt%, and most preferably less than or equal to 0.005 wt%.
In the invention, the preferred specific surface area of the titanium dioxide for the plastic color master batch is 13-15 m2A more preferable range is 13.5 to 14.5 m/g2/g。
In the invention, the volatile matter of the titanium dioxide powder for the plastic color master batch after being dried for 2 hours at 105 ℃ is preferably less than or equal to 0.2 wt%, and more preferably less than or equal to 0.1 wt%.
In the invention, the plastic color master batch is dried by titanium dioxide at 105 ℃ for 2h, and the ignition loss after ignition for 1h at 900 ℃ is preferably less than or equal to 0.3 wt%, and more preferably less than or equal to 0.2 wt%.
The invention provides a preparation method of titanium dioxide for plastic color master batches, which preferably comprises the following steps:
(1) adding ammonia water into the concentrated titanium solution until the pH value of the obtained mixed material is 2.4-2.6, heating the mixed material to 88-92 ℃ at the heating rate of 4.5-5.5 ℃/min, and preserving the heat for 4.5-5.5 min to obtain hydrolysis crystal seeds; wherein the process of adding ammonia water is controlled to be completed within 9-11 min;
(2) mixing the hydrolysis seed crystal in the step (1) with the concentrated titanium liquid at the temperature of 95-97 ℃, and hydrolyzing to obtain hydrolysis metatitanic acid slurry;
(3) washing the hydrolyzed metatitanic acid slurry obtained in the step (2) to obtain washed metatitanic acid slurry;
(4) adding calcined rutile type seed crystal, ZnO and NH into the washed metatitanic acid slurry in the step (3) in sequence4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Carrying out salt treatment to obtain salt-treated metatitanic acid slurry;
(5) filtering the salt-treated metatitanic acid slurry obtained in the step (4), and calcining the filtered solid material to obtain a crude product material;
(6) and (5) crushing and surface treating the crude product material in the step (5) to obtain the titanium dioxide for the plastic color master batch.
According to the method, ammonia water is preferably added into the concentrated titanium solution until the pH value of the obtained mixed material is 2.4-2.6, the mixed material is heated to 88-92 ℃ at the heating rate of 4.5-5.5 ℃/min, and the temperature is kept for 4.5-5.5 min, so that hydrolysis crystal seeds are obtained; wherein the process of adding ammonia water is controlled to be completed within 9-11 min. In the invention, the mass percentage of the ammonia water is preferably 18-22%, and more preferably 20%.
In the present invention, the index of the concentrated titanium solution is preferably: TiO 22The content is more than or equal to 205 +/-3 g/L, Ti3+The content is 1.0-2.0 g/L, and the F value is 2.02.1, the iron-titanium ratio is 0.42-0.45, the stability is more than or equal to 500, and the clarity is qualified. In the stability test method, 1mL of solution to be tested is diluted until a milky white substance (metatitanic acid) appears after 20s of the obtained diluted solution is taken as a stability test endpoint; the stability was evaluated by fold dilution. In the invention, specifically, 1mL of concentrated titanium solution is diluted to at least 500mL, and after the obtained diluted titanium solution appears a milky substance after 20s, the stability of the concentrated titanium solution is more than or equal to 500.
The source of the concentrated titanium solution is not particularly limited in the present invention, and the concentrated titanium solution prepared by a method known to those skilled in the art may be used. In the present invention, the method for preparing the concentrated titanium solution preferably includes the steps of:
(a) mixing titanium ore and concentrated sulfuric acid for acidolysis, and performing heat preservation and curing to obtain an acidolysis solid-phase substance; the mass percentage content of the concentrated sulfuric acid is 83-87%;
(b) mixing the acidolysis solid-phase substance in the step (a) with dilute sulfuric acid for leaching to obtain leaching solution; the mass percentage of the dilute sulfuric acid is 25-30%;
(c) mixing the leaching solution in the step (b) with iron powder for reduction reaction to obtain a reducing solution;
(d) mixing the reducing solution in the step (c) with a settling agent for settling to obtain a supernatant as a titanium solution;
(e) and (d) crystallizing, filtering and concentrating the titanium liquid obtained in the step (d) in sequence to obtain a concentrated titanium liquid.
In the invention, the titanium ore and concentrated sulfuric acid are preferably mixed for acidolysis, and the mixture is subjected to heat preservation and curing to obtain an acidolysis solid-phase substance; the mass percentage of the concentrated sulfuric acid is 83-87%. In the present invention, the indexes of the titanium ore are preferably: with TiO2The titanium content is 40-50%, the rutile content is less than or equal to 3%, the high-iron content is less than or equal to 13%, the total content of ferrous and high-iron is greater than or equal to 94%, and the colloidal impurity content is less than or equal to 3%. The invention preferably crushes the titanium ore to obtain ore powder with the fineness of 320 meshes, and then mixes the ore powder with concentrated sulfuric acid for acidolysis; more preferably, the titanium ore is crushed to the fineness of 320 meshes by a horizontal ball mill and the surplus is sievedThe substance is less than or equal to 3.5 percent, and the mineral powder is obtained. In the invention, the mass percentage of the concentrated sulfuric acid is preferably 84-86%, and more preferably 85%.
The mineral powder is preferably mixed with sulfuric acid with the mass percentage of 96-98%, and then water is added for acidolysis, wherein the process of adding water is completed within 3 min. In the invention, the mass ratio of the mineral powder to 96-98% sulfuric acid is preferably 1: (1.5 to 1.7), more preferably 1: 1.6. The addition amount of the water is not particularly limited, and the sulfuric acid concentration can be ensured to meet the acidolysis condition. In the invention, the time for acidolysis is calculated by the violent reaction starting 7-9 min after the water is added, and the time for acidolysis is preferably 2.5-3.5 min, and more preferably 3 min. In the invention, the temperature of the heat preservation curing is preferably 80-100 ℃, more preferably 85-95 ℃, and most preferably 90 ℃; the time for heat preservation and curing is preferably 120-140 min, more preferably 125-135 min, and most preferably 130 min. In the present invention, the incubation aging is preferably performed by steam heating. In the invention, after the acidolysis is finished, the reactant is gradually thickened to form a solid-phase substance, the heat preservation and the curing are carried out through steam heating, the sulfuric acid decomposition reaction can be continuously carried out, and the improvement of the sulfuric acid decomposition rate is facilitated.
After the acidolysis solid-phase substance is obtained, the acidolysis solid-phase substance is preferably mixed with dilute sulfuric acid for leaching to obtain leaching solution; the mass percentage of the dilute sulfuric acid is 25-30%. The acidolysis solid-phase substance is preferably mixed with sulfuric acid with the mass percentage of 15-20%, and then water is added for leaching to obtain a leaching solution; wherein the process of adding water is controlled to be completed within 30-40 min. In the present invention, the index of the obtained leaching solution is preferably: TiO 22The content is 120-135 g/L, the specific gravity is 48-51, and the F value is 1.85-2.05. In the invention, after the acid hydrolysis is finished, the obtained acid hydrolysis solid-phase substance contains free sulfuric acid, the acid hydrolysis solid-phase substance is mixed with sulfuric acid with the mass percentage of 15-20%, water is added to form a liquid phase system, the free sulfuric acid contained in the acid hydrolysis solid-phase substance is dissolved in the formed liquid phase system, and finally the sulfur in the obtained liquid phase system is dissolvedAnd (3) leaching the acid with the mass percentage of 25-30%. In the invention, the addition amount of the sulfuric acid and the water with the mass percentage content of 15-20% needs to make the mass percentage content of the sulfuric acid in the liquid phase system in the leaching process be 25-30% on one hand, and make the leaching solution obtained after the leaching meet the indexes on the other hand. In the embodiment of the invention, the sulfuric acid with the mass percentage of 15-20% preferably adopts industrial waste acid. In the invention, the leaching temperature is preferably 55-65 ℃, more preferably 58-62 ℃, and most preferably 60 ℃; the leaching time is preferably 5-12 hours, more preferably 7-10 hours, and most preferably 8 hours.
After the leaching solution is obtained, the leaching solution and the iron powder are preferably mixed for reduction reaction to obtain a reduction solution. The iron powder of the present invention is not particularly limited, and iron powder for carrying out reduction reaction, which is well known to those skilled in the art, may be used. In the invention, the addition amount of the iron powder can ensure that the ferric iron in the leaching solution is reduced into ferrous iron. The iron powder is preferably added into the leaching solution, wherein the process of adding the iron powder is controlled to be completed within 20-30 min, and the temperature is less than or equal to 75 ℃. In the invention, the time of the reduction reaction is preferably 8-12 min, and more preferably 10 min. In the invention, the reduction reaction is started when the iron powder is added, and the time of the reduction reaction is counted by the time when the iron powder is added.
After the reducing solution is obtained, the reducing solution and a settling agent are preferably mixed for settling, and the obtained supernatant is used as the titanium solution. The invention has no special limitation on the type of the settling agent, and the settling agent which is well known to a person skilled in the art can be adopted; in the examples of the present invention, Sb is specifically used2O3And FeS as a settling agent. In the present invention, the Sb is2O3And FeS are preferably in a mass ratio of 1: (1.8-2.2), more preferably 1: 2. In the present invention, TiO is used2Meter, the Sb2O3The total mass of FeS and FeS is preferably 1-4 per mill of the mass of the reducing liquid, and more preferably 2-3 per mill. In the present invention, the Sb is2O3Preferably Sb2O3In the form of hydrochloric acid solution, the Sb2O3The concentration of the hydrochloric acid solution is preferably 1.4-1.6 kg/L, and more preferably 1.5 kg/L; the FeS is directly prepared from solid FeS. In the invention, Sb is preferably added into the reducing solution in sequence2O3Settling hydrochloric acid solution and FeS to obtain supernatant serving as titanium liquid; wherein Sb is added2O3The process of the hydrochloric acid solution is controlled to be completed within 2.5-3.5 min, and the process of adding the FeS solution is controlled to be completed within 4.5-5.5 min. In the invention, the settling time is preferably 2-4 h, and more preferably 3 h. The purpose of sedimentation in the present invention is to remove insoluble impurities, particularly colloids, from the reducing solution.
After obtaining the titanium solution, the invention preferably performs crystallization, filtration and concentration on the titanium solution in sequence to obtain the concentrated titanium solution. The crystallization is not particularly limited in the invention, and the technical scheme of crystallization well known to those skilled in the art can be adopted; vacuum crystallization is preferred for the present invention. In the present invention, the degree of vacuum of the vacuum crystallization is preferably 0.0095 to 0.001MPa, and more preferably 0.0098 MPa. The vacuum crystallization is used for removing ferrous sulfate in the titanium liquid so that the titanium liquid can meet the requirement of the subsequent hydrolysis step. The invention has no special limitation on the filtration, and the technical scheme of filtration known by the technicians in the field can be adopted; in the invention, the filter cloth adopted in the filtration is preferably 120-150 meshes. In the present invention, the filtration is performed to purify the crystallized titanium solution obtained after the crystallization to further remove impurities such as colloids and slurry. The concentration is not particularly limited in the invention, and the technical scheme of concentration well known to those skilled in the art can be adopted; in the invention, the concentration temperature is preferably 40-50 ℃, more preferably 45 ℃, and the vacuum degree of the concentration is preferably 0.08-0.1 MPa, more preferably 0.09 MPa.
After obtaining the hydrolysis seed crystal, the hydrolysis seed crystal is preferably mixed with the concentrated titanium liquid at the temperature of 95-97 ℃ for hydrolysis, so as to obtain the hydrolysis metatitanic acid slurry. In the present invention, the index of the concentrated titanium solution is preferably: TiO 22The content is more than or equal to 205 +/-3 g/L, Ti3+The content is 1.0 to 2.0g/L,f value is 2.0-2.1, iron-titanium ratio is 0.42-0.45, stability is more than or equal to 500, and clarity is qualified. In the invention, the mass ratio of the concentrated titanium solution required for preparing the hydrolyzed metatitanic acid slurry to the concentrated titanium solution required for preparing the hydrolysis seed crystal is preferably 1: (8.5 to 9.5), and more preferably 1: 9. In the present invention, the hydrolysis preferably comprises the steps of:
mixing the hydrolysis crystal seeds with the concentrated titanium liquid at the temperature of 95-97 ℃, heating the steam to the first boiling within 28min, stopping the steam, and preserving the heat for 25-35 min to obtain a first boiling material;
at 90-120 mmH2Heating the first boiling material steam to a second boiling state within 20min under O, and maintaining the pressure for 140-160 min to obtain a second boiling material;
diluting the second boiling material to TiO2The content of the additive is 155-165 g/L and is 90-120 mmH2And (4) heating the steam to a third boiling point within 10min under the condition of O, and maintaining the pressure for 8-12 min to obtain the hydrolyzed metatitanic acid slurry.
According to the invention, the hydrolysis crystal seeds are preferably mixed with the concentrated titanium liquid at the temperature of 95-97 ℃, steam is heated to the first boiling within 28min, and the steam is stopped and the temperature is kept for 25-35 min to obtain the first boiling material. According to the invention, preferably, hydrolysis seed crystals are added into the concentrated titanium solution at the temperature of 95-97 ℃; wherein the process of adding the hydrolysis seed crystal is controlled to be completed within 5 min. In the invention, after the steam is heated to the first boiling, the invention preferably detects the obtained material to determine the time for stopping the steam; specifically, 5mL of the material is mixed with 10mL of water, and when the obtained mixed material generates a milky white substance (metatitanic acid), steam can be stopped.
After the first boiling material is obtained, the optimal selection of the boiling material is 90-120 mmH2And heating the first boiling material steam to a second boiling state within 20min under the condition of O, and maintaining the pressure for 140-160 min to obtain a second boiling material. In the invention, the pressure of steam heating to the second boiling is preferably 100-110 mmH2O; the pressure maintaining time is preferably 145-155 min.
After obtaining the second boiling material, the present invention preferably dilutes the second boiling material to TiO2The content of the additive is 155-165 g/L and is 90-120 mmH2Heating with steam for 10min to thirdBoiling and maintaining the pressure for 8-12 min to obtain the hydrolyzed metatitanic acid slurry. The invention preferably mixes the second boiling material with water to dilute the second boiling material to TiO2The content is 155-165 g/L. In the invention, the pressure of steam heating to the third boiling is preferably 100-110 mmH2O。
After the hydrolysis is completed, the present invention preferably mixes the obtained material with a filter aid to obtain a hydrolyzed metatitanic acid slurry. The amount of the filter aid used in the present invention is not particularly limited, and may be any amount known to those skilled in the art. The filter aid of the present invention is not particularly limited in kind, and may be one known to those skilled in the art. In the examples of the present invention, lignocellulose is used in particular as a filter aid. In the invention, the filter aid is beneficial to the subsequent washing step, and the impurity content of the washing metatitanic acid slurry is less than 20PP (calculated by ferric oxide).
After obtaining the hydrolyzed metatitanic acid slurry, the invention preferably washes the hydrolyzed metatitanic acid slurry to obtain the washed metatitanic acid slurry. The washing method of the present invention is not particularly limited, and a washing method known to those skilled in the art may be used. In the present invention, the washing preferably includes water washing and rinsing, which are sequentially performed. In the invention, the washing temperature is preferably 70-80 ℃, and more preferably 75 ℃; the time of the water washing is preferably 2.5-3.5 h, and more preferably 3 h. After the washing is finished, the obtained washing material is preferably filtered, the obtained filter cake is mixed with water, and TiO in the obtained washing material is enabled to be in2The content is 290-310 g/L, and then rinsing is carried out.
In the invention, the rinsing is preferably carried out by mixing the water-washed material, concentrated sulfuric acid and aluminum powder, heating the mixture to 85-95 ℃ by steam, and keeping the temperature for 1-2 hours to obtain the washing metatitanic acid slurry. In the invention, the mass percentage of the concentrated sulfuric acid is preferably 96-98%; the purity of the aluminum powder is preferably more than 99.9%; with TiO2The mass ratio of the water washing material to the concentrated sulfuric acid to the aluminum powder is preferably 6 (0.9-1.1): (0.55-0.65%). More preferably 6: 1: 0.6 percent. The invention is preferably carried out by rinsingControlling Fe in the obtained washing metatitanic acid slurry2+In an amount of<10ppm，Ti3+The content of (C) is (0.5-0.7) g/L. If rinsed once, Fe2 +The content of (b) is not enough to meet the above requirements, and secondary rinsing can be performed according to actual conditions.
After obtaining the washing metatitanic acid slurry, the invention preferably adds the calcined rutile type seed crystal, ZnO and NH into the washing metatitanic acid slurry in sequence4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3And carrying out salt treatment to obtain the salt-treated metatitanic acid slurry. In the invention, the mass of the washed metatitanic acid slurry and the calcined rutile type seed crystal is TiO2Meter, NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Respectively with the mass of P2O5、K2O、Al2O3And Ce2O3Washing metatitanic acid slurry, and calcining rutile type seed crystal, ZnO and NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Is preferably 100: (7-18): (0.10-0.16), (1-2), (1.3-2.5), (1-8): (0.05 to 0.10), more preferably 100: (10-15): (0.11-0.15), (1.3-1.7), (1.6-2.2), (3-6): (0.06-0.09), most preferably 100: (12-13): (0.12-0.13), (1.4-1.6), (1.8-2.0), (4-5): (0.07-0.08). In the invention, the mass percentage of the KOH solution is preferably 35-45%, and more preferably 40%.
In the present invention, the method for preparing the calcined rutile type seed crystal preferably comprises the steps of:
adding washing metatitanic acid slurry at 109-111 ℃ into a sodium hydroxide solution at 104-106 ℃ to obtain a mixed system, wherein the process of adding the washing metatitanic acid slurry is controlled to be completed within 15-20 min;
heating the mixed system to 120-130 ℃ by steam, and preserving heat for 35-45 min to obtain sodium orthotitanate slurry;
sequentially neutralizing and washing the sodium orthotitanate slurry to obtain an orthotitanate slurry;
heating the orthotitanic acid slurry to 59-61 ℃ by steam, adding hydrochloric acid until the pH value of the obtained material is 1.0-1.2, heating the material to 102-104 ℃ at a heating rate of 0.8-1.2 ℃/min, preserving heat for 55-65 min, and cooling to 40-50 ℃ in 30min to obtain the calcined rutile type seed crystal.
According to the invention, the washing metatitanic acid slurry at 109-111 ℃ is preferably added into the sodium hydroxide solution at 104-106 ℃ to obtain a mixed system, wherein the process of adding the washing metatitanic acid slurry is controlled to be completed within 15-20 min. In the invention, the mass percentage of the NaOH solution is preferably 48-52%, and more preferably 50%; with TiO2The mass ratio of the washing metatitanic acid slurry to the NaOH solution is preferably 1: (1.4-1.6), and more preferably 1: 1.5.
After a mixed system is obtained, the mixed system is preferably heated to 120-130 ℃ by steam, and the temperature is kept for 35-45 min to obtain the sodium orthotitanate slurry. In the invention, the steam heating temperature is preferably 122-128 ℃, and more preferably 125 ℃; the heat preservation time is preferably 38-42 min, and more preferably 40 min.
After obtaining the sodium orthotitanate slurry, the invention preferably performs neutralization and washing on the sodium orthotitanate slurry in sequence to obtain the sodium orthotitanate slurry. Before the neutralization, the invention preferably removes a large amount of free sodium hydroxide in the sodium titanate slurry; specifically, the sodium orthotitanate slurry is mixed with water, cooled to 50-60 ℃, filtered, and the obtained filtrate can be industrially used for tail gas spraying, and the obtained filter cake is pulped and then neutralized. In the present invention, the mass ratio of the sodium orthotitanate slurry to water is preferably 10: (2.5-3.5), more preferably 10: 3. The present invention is not particularly limited to the neutralization and washing, and the neutralization and washing method known to those skilled in the art may be used. In the invention, the filter cake is pulped, neutralized by 8-12% by mass of hydrochloric acid until the pH value is 3.5-4.0, washed until the pH value of the filtrate is 5.5-7, and the obtained filter cake is beatenObtaining orthotitanic acid slurry after pulping; TiO in the orthotitanic acid slurry2The content of (b) is preferably 200 to 220g/L, more preferably 210 g/L. In the invention, after the filter cake is pulped, the filter cake is neutralized by hydrochloric acid with the mass percentage of 8-12% until the pH value is 3.5-4.0, and then the filter cake is washed until the pH value of the filtrate is 5.5-7, so that sodium ions can be removed.
After obtaining the orthotitanic acid slurry, the invention preferably heats the orthotitanic acid slurry to 59-61 ℃ by steam, adds hydrochloric acid until the pH value of the obtained material is 1.0-1.2, heats the material to 102-104 ℃ at a heating rate of 0.8-1.2 ℃/min, keeps the temperature for 55-65 min, and cools to 40-50 ℃ in 30min to obtain the calcined rutile type seed crystal. In the invention, the mass percentage of the hydrochloric acid is preferably 25-35%, and more preferably 30%. In the present invention, TiO in the calcined rutile seed crystal2The content of (b) is preferably 90 to 100 g/L. The calcined rutile type seed crystal prepared by the method provided by the invention has high activity, fine particle size and narrow distribution, less addition amount and high rutile conversion rate of the product.
In the invention, the salt treatment time is preferably 2.5-3.5 h, and more preferably 3 h. In the present invention, the salt treatment is preferably carried out under mechanical stirring conditions; the mechanical stirring is not specially limited, and the materials can be mixed and uniformly dispersed.
After obtaining the salt-treated metatitanic acid slurry, the invention preferably filters the salt-treated metatitanic acid slurry, and calcines the solid material obtained by filtering to obtain a crude product material. The present invention is not particularly limited to the above filtration, and a filtration technique known to those skilled in the art may be used. In the present invention, the calcination preferably includes a first calcination and a second calcination performed in this order; the temperature of the first calcination is preferably 450-600 ℃, and more preferably 500-550 ℃; the first calcination time is preferably 6-8 h, and more preferably 7 h; the second calcining temperature is preferably 700-900 ℃, and more preferably 750-850 ℃; the second calcination time is preferably 8-10 h, and more preferably 9 h. By adopting the calcination method provided by the invention, the obtained titanium dioxide is not easy to sinter, and has good whiteness and brightness.
After a crude product material is obtained, the invention preferably performs crushing and surface treatment on the crude product material to obtain the titanium dioxide for the plastic color master batch. In the present invention, the pulverization and the surface treatment preferably include the steps of:
mixing the crude product material with aluminum hydroxide gel, and performing first crushing to obtain a first crushed material with the particle size of 0.6-45 mu m;
performing second crushing on the first crushed material to obtain a second crushed material with the particle size of 0.3-0.5 mu m;
and mixing the second crushed material with trimethylchlorosilane, and performing third crushing to obtain the titanium dioxide for the plastic color master batch with the particle size of 0.23-0.27 mu m.
Mixing the crude product material with aluminum hydroxide gel, and performing first crushing to obtain a first crushed material with the particle size of 0.6-45 mu m. In the present invention, TiO is used2In terms of mass ratio, the mass ratio of the crude product material to the aluminum hydroxide gel is preferably 1 (0.8-1.6%), and more preferably 1 (1.0-1.2%). In the present invention, the particle size of the aluminum hydroxide gel is preferably 1.5 to 2.5 μm, and more preferably 1.8 to 2.2 μm. The first pulverization is preferably carried out by a first-grade Raymond mill.
After the first crushed material is obtained, the first crushed material is preferably subjected to second crushing to obtain a second crushed material with the particle size of 0.3-0.5 mu m. The present invention preferably employs a micron mill for the second pulverization.
After the second crushed material is obtained, the second crushed material is preferably mixed with trimethylchlorosilane for third crushing to obtain the titanium dioxide for the plastic color master batch with the particle size of 0.23-0.27 mu m. In the present invention, TiO is used2Preferably, the mass ratio of the second crushed material to the trimethylchlorosilane is 1: (0.8 to 1.2%), and more preferably 1: 1%. The present invention preferably performs the third pulverization using a jet mill.
After the crushing and the surface treatment are finished, the obtained materials are preferably subjected to dust removal, finished product collection and packaging in sequence to obtain the titanium dioxide product for the plastic color master batch. The dust removal, finished product collection and packaging are not particularly limited in the invention, and related technical schemes well known to those skilled in the art can be adopted.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Selecting raw ore, wherein the indexes are as follows: with TiO2The titanium content is 40-50%, the rutile content is less than or equal to 3%, the high-iron content is less than or equal to 13%, the total content of ferrous and high-iron is greater than or equal to 94%, and the colloidal impurity content is less than or equal to 3%; crushing raw ore to the fineness of 320 meshes by adopting a horizontal ball mill, wherein the sieve residue is less than or equal to 3.5 percent, and obtaining ore powder;
(2) under the stirring of compressed air, mixing 30t of mineral powder with 90.12t of sulfuric acid with the mass percentage content of 98%, stirring for 10min, adding 14.1t of water within 3min, continuously stirring for 8min to start violent reaction, calculating the acidolysis time, heating steam to 90 ℃ after acidolysis for heat preservation and curing for 130min after 3min of acidolysis, and obtaining an acidolysis solid-phase substance;
(3) mixing the acidolysis solid-phase substance with 3000mL of waste acid under the stirring of compressed air, adding 60t of water at the speed of 100t/h, and leaching at 60 ℃ for 8h to obtain a leaching solution; the indexes of the leaching solution are as follows: TiO 22The content is 130g/L, the specific gravity is 50, and the F value is 1.95;
(4) adding 1.2t of iron powder into the leaching solution, wherein the process of adding the iron powder is controlled to be 25min, the temperature is controlled to be 70 ℃, and reduction reaction is carried out for 10min to obtain reducing solution;
(5) adding 1.5kg/L Sb into the reducing solution2O350L of hydrochloric acid solution, adding for 3min, stirring with compressed air for 10min, adding 200kg of FeS for 5min, and stirring with compressed airStirring for 10min, standing for 2h, and settling to obtain clear solution as titanium solution;
(6) performing vacuum crystallization on the titanium liquid under the condition that the vacuum degree is 0.0098MPa, filtering the obtained material, and concentrating the filtrate at 45 ℃ under the condition of 0.09MPa to obtain concentrated titanium liquid; the indexes of the concentrated titanium solution are as follows: TiO 22Is 205g/L, Ti3+1.5g/L, F value of 2.05, iron-titanium ratio of 0.43, stability of 500 and clarity of qualified product;
(7) adding ammonia water with the mass percentage of 20% into the concentrated titanium solution until the pH value of the obtained mixed material is 2.5, heating the mixed material to 90 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 5min to obtain hydrolysis crystal seeds; wherein the adding time of the ammonia water is controlled to be 10 min;
(8) adding hydrolysis seed crystals into the 96 ℃ concentrated titanium solution, wherein the adding time is controlled within 5min, and the mass ratio of the 96 ℃ concentrated titanium solution to the concentrated titanium solution required for preparing the hydrolysis seed crystals is 1: 9; heating the steam to the first boiling within 28min, stopping the steam and preserving the heat for 30min when the obtained material meets the requirement through detection, thus obtaining a first boiling material; the detection method comprises the steps of mixing 5mL of material with 10mL of water, and stopping steam when the obtained mixed material is milky white;
at 100mmH2Heating the first boiling material steam to a second boiling state within 20min under O, and maintaining the pressure for 150min to obtain a second boiling material;
adding water to dilute the second boiling material to TiO2The content is 160g/L and is 100mmH2Heating the steam to a third boiling point within 5min under O, maintaining the pressure for 10min, adding lignocellulose under mechanical stirring, and stirring for 10min to obtain hydrolysis metatitanic acid slurry;
(9) washing the hydrolyzed metatitanic acid slurry for 3h at 75 ℃, filtering, and mixing the obtained filter cake with water to obtain TiO2Washing the material with water at a content of 300g/L with TiO2According to the mass ratio of the water washing material to the concentrated sulfuric acid to the aluminum powder of 6: 1: 0.6 percent of washing material, adding 98 percent of sulfuric acid and 99.9 percent of aluminum powder by mass percentage into the washing material, heating the mixture to 90 ℃ by steam, and preserving the heat for 1.5 hours to obtain washing metatitanic acid slurry; the washing is carried outIndexes of the poly (metatitanic acid) slurry are as follows: fe2+In an amount of<10ppm，Ti3+The content of (A) is 0.6 g/L;
(10) adding metatitanic acid slurry at 110 ℃ into sodium hydroxide solution with the mass percentage of 50% at 105 ℃ to obtain a mixed material; the adding time of the metatitanic acid slurry is controlled to be 15 min; with TiO2The mass ratio of the metatitanic acid slurry to the NaOH solution is 1: 1.5;
heating the mixed material to 125 ℃ by steam, and preserving the heat for 40min to obtain sodium orthotitanate slurry;
mixing the sodium orthotitanate slurry with water according to the mass ratio of the sodium orthotitanate slurry to the water of 10:3, cooling to 50-60 ℃, filtering, pulping the obtained filter cake, neutralizing with 10% hydrochloric acid by mass percentage until the pH value is 3.5-4.0, washing until the pH value of the filtrate is 5-6, and pulping the obtained filter cake to obtain the sodium orthotitanate slurry; TiO in the orthotitanic acid slurry2The content of (A) is 210 g/L;
heating the orthotitanic acid slurry to 60 ℃ by steam, adding hydrochloric acid with the mass percentage of 30% until the pH value of the obtained material is 1.0-1.2, heating the material to 103 ℃ at the heating rate of 1 ℃/min, preserving the heat for 60min, and cooling to 45 ℃ in 30min to obtain calcined rutile type crystal seeds; TiO in the calcined rutile type seed crystal2The content of (A) is 95 g/L;
adding calcined rutile type seed crystal, ZnO and NH into the washing metatitanic acid slurry in sequence4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Carrying out salt treatment for 3h under mechanical stirring to obtain salt-treated metatitanic acid slurry; wherein the mass of the washing metatitanic acid slurry and the calcined rutile type seed crystal is TiO2Meter, NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Respectively with the mass of P2O5、K2O、Al2O3And Ce2O3Washing metatitanic acid slurry, and calcining rutile type seed crystal, ZnO and NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3The mass ratio of (A) to (B) is 100: 12: 0.12:1.5:1.9:4.5: 0.07;
(11) filtering the salt-treated metatitanic acid slurry, and performing first calcination on the obtained solid material at 500 ℃ for 7 hours, and then performing second calcination at 800 ℃ for 9 hours to obtain a crude product material;
(12) mixing the crude product material with aluminum hydroxide gel with the particle size of 1.5-2.5 mu m, and performing first crushing by adopting a first-level Raymond machine to obtain a first crushed material with the particle size of 0.6-45 mu m; wherein, TiO is used2The mass ratio of the crude product material to the aluminum hydroxide gel is 1: 1.1%;
performing second crushing on the first crushed material by using a micron crusher to obtain a second crushed material with the particle size of 0.3-0.5 mu m;
mixing the second crushed material with trimethylchlorosilane, and performing third crushing by using a jet mill to obtain titanium dioxide for plastic color master batch with the particle size of 0.23-0.27 mu m, wherein TiO is used2And the mass ratio of the second crushed material to the trimethylchlorosilane is 1: 1%.
The performance index analysis is carried out on the prepared titanium dioxide for the plastic color master batch, and the result is as follows:
TiO2the content of rutile type TiO is 97.5%2The content is 99.7%;
Al2O3the content is 0.8%;
the content of the trimethylchlorosilane is 0.7 percent;
Fe2O3the content is 0.005%;
specific surface area of 15m2/g；
Particle diameter D500.23 to 0.27 μm, particle diameter D99≤0.5μm；
0.005% of 45 mu m screen residue;
the volatile matter (105 ℃, 2h) is 0.2 percent;
the ignition loss (105 ℃, 2h after drying, 900 ℃ ignition for 1h) is 0.3%;
the pH value of the aqueous suspension is 7.0;
hue: the L value is 98.5%, the b value is 1.4, and the a value is 0.3;
the decolorization rate is 110 percent;
the dispersity is 7.0;
the water absorption capacity is 35g/50 g;
the oil absorption was 11g/100 g.
Example 2
(1) Selecting raw ore, wherein the indexes are as follows: with TiO2The titanium content is 40-50%, the rutile content is less than or equal to 3%, the high-iron content is less than or equal to 13%, the total content of ferrous and high-iron is greater than or equal to 94%, and the colloidal impurity content is less than or equal to 3%; crushing raw ore to the fineness of 320 meshes by adopting a horizontal ball mill, wherein the sieve residue is less than or equal to 3.5 percent, and obtaining ore powder;
(2) mixing 30t of mineral powder and 90.12t of sulfuric acid with the mass percentage content of 98% under the stirring of compressed air, stirring for 10min, adding 14.1t of water within 3min, continuously stirring for 8min to start violent reaction, calculating the acidolysis time, heating steam to 80 ℃ after acidolysis for 140min, and carrying out heat preservation and curing to obtain an acidolysis solid-phase substance;
(3) mixing the acidolysis solid-phase substance with 3000mL of waste acid under the stirring of compressed air, adding 60t of water at the speed of 100t/h, and leaching at 65 ℃ for 6h to obtain a leaching solution; the indexes of the leaching solution are as follows: TiO 22The content is 120g/L, the specific gravity is 49, and the F value is 1.85;
(4) adding 1.2t of iron powder into the leaching solution, wherein the process of adding the iron powder is controlled to be 25min, the temperature is controlled to be 65 ℃, and a reduction reaction is carried out for 12min to obtain a reduction solution;
(5) adding 1.5kg/L Sb into the reducing solution2O350L of hydrochloric acid solution, wherein the adding time is controlled to be 3min, the compressed air is stirred for 10min after the adding is finished, then 200kg of FeS is added, the adding time is controlled to be 5min, the compressed air is stirred for 10min after the adding is finished, and clear solution obtained after the settling is kept for 3h and is used as titanium liquid;
(6) vacuum crystallizing the titanium liquid under the condition that the vacuum degree is 0.0098MPa, filtering the obtained material, and concentrating the filtrate under the conditions of 45 ℃ and 0.09MPaCondensing to obtain concentrated titanium liquid; the indexes of the concentrated titanium solution are as follows: TiO 22Is 205g/L, Ti3+1.3g/L, F value of 2.0, iron-titanium ratio of 0.44, stability of 500 and clarity of qualified product;
(7) adding ammonia water with the mass percentage of 20% into the concentrated titanium solution until the pH value of the obtained mixed material is 2.5, heating the mixed material to 90 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 5min to obtain hydrolysis crystal seeds; wherein the adding time of the ammonia water is controlled to be 10 min;
(8) adding hydrolysis seed crystals into the 96 ℃ concentrated titanium solution, wherein the adding time is controlled within 5min, and the mass ratio of the 96 ℃ concentrated titanium solution to the concentrated titanium solution required for preparing the hydrolysis seed crystals is 1: 9; heating the steam to the first boiling within 28min, stopping the steam and preserving the heat for 35min when the obtained material meets the requirement through detection, thus obtaining a first boiling material; the detection method comprises the steps of mixing 5mL of material with 10mL of water, and stopping steam when the obtained mixed material is milky white;
at 110mmH2Heating the first boiling material steam to a second boiling state within 20min under O, and maintaining the pressure for 160min to obtain a second boiling material;
adding water to dilute the second boiling material to TiO2The content is 160g/L and is 110mmH2Heating the steam to a third boiling point within 5min under O, maintaining the pressure for 10min, adding lignocellulose under mechanical stirring, and stirring for 10min to obtain hydrolysis metatitanic acid slurry;
(9) washing the hydrolyzed metatitanic acid slurry for 3h at 70 ℃, filtering, and mixing the obtained filter cake with water to obtain TiO2Washing the material with water at a content of 300g/L with TiO2According to the mass ratio of the water washing material to the concentrated sulfuric acid to the aluminum powder of 6: 1: 0.6 percent of washing material, adding 98 percent of sulfuric acid and 99.9 percent of aluminum powder by mass percentage into the washing material, heating the mixture to 90 ℃ by steam, and preserving the heat for 1.5 hours to obtain washing metatitanic acid slurry; indexes of the washing metatitanic acid slurry are as follows: fe2+In an amount of<10ppm，Ti3+The content of (A) is 0.6 g/L;
(10) adding metatitanic acid slurry at 110 ℃ into sodium hydroxide solution with the mass percentage of 50% at 105 DEG CFeeding to obtain a mixed material; the adding time of the metatitanic acid slurry is controlled to be 15 min; with TiO2The mass ratio of the metatitanic acid slurry to the NaOH solution is 1: 1.5;
heating the mixed material to 125 ℃ by steam, and preserving the heat for 40min to obtain sodium orthotitanate slurry;
mixing the sodium orthotitanate slurry with water according to the mass ratio of the sodium orthotitanate slurry to the water of 10:3, cooling to 50-60 ℃, filtering, pulping the obtained filter cake, neutralizing with 10% hydrochloric acid by mass percentage until the pH value is 3.5-4.0, washing until the pH value of the filtrate is 5-6, and pulping the obtained filter cake to obtain the sodium orthotitanate slurry; TiO in the orthotitanic acid slurry2The content of (A) is 210 g/L;
heating the orthotitanic acid slurry to 60 ℃ by steam, adding hydrochloric acid with the mass percentage of 30% until the pH value of the obtained material is 1.0-1.2, heating the material to 103 ℃ at the heating rate of 1 ℃/min, preserving the heat for 60min, and cooling to 45 ℃ in 30min to obtain calcined rutile type crystal seeds; TiO in the calcined rutile type seed crystal2The content of (A) is 95 g/L;
adding calcined rutile type seed crystal, ZnO and NH into the washing metatitanic acid slurry in sequence4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Carrying out salt treatment for 3h under mechanical stirring to obtain salt-treated metatitanic acid slurry; wherein the mass of the washing metatitanic acid slurry and the calcined rutile type seed crystal is TiO2Meter, NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Respectively with the mass of P2O5、K2O、Al2O3And Ce2O3Washing metatitanic acid slurry, and calcining rutile type seed crystal, ZnO and NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3The mass ratio of (A) to (B) is 100: 13: 0.13:1.6:2.0:4.8: 0.08;
(11) filtering the salt-treated metatitanic acid slurry, and performing first calcination on the obtained solid material at 550 ℃ for 6 hours, and then performing second calcination at 850 ℃ for 8 hours to obtain a crude product material;
(12) mixing the crude product material with aluminum hydroxide gel with the particle size of 1.5-2.5 mu m, and performing first crushing by adopting a first-level Raymond machine to obtain a first crushed material with the particle size of 0.6-45 mu m; wherein, TiO is used2The mass ratio of the crude product material to the aluminum hydroxide gel is 1: 1.2%;
performing second crushing on the first crushed material by using a micron crusher to obtain a second crushed material with the particle size of 0.3-0.5 mu m;
mixing the second crushed material with trimethylchlorosilane, and performing third crushing by using a jet mill to obtain titanium dioxide for plastic color master batch with the particle size of 0.23-0.27 mu m, wherein TiO is used2And the mass ratio of the second crushed material to the trimethylchlorosilane is 1: 1.1%.
The performance index analysis is carried out on the prepared titanium dioxide for the plastic color master batch, and the result is as follows:
TiO2the content of rutile type TiO is 98.5 percent2The content is 99.5%;
Al2O3the content is 0.9%;
the content of the trimethylchlorosilane is 0.8 percent;
Fe2O3the content is 0.004%;
specific surface area 14m2/g；
Particle diameter D500.23 to 0.27 μm, particle diameter D99≤0.5μm；
0.008% of 45 mu m screen residue;
the volatile matter (105 ℃, 2h) is 0.15 percent;
the ignition loss (105 ℃, 2h after drying, 900 ℃ ignition for 1h) is 0.25%;
the pH value of the aqueous suspension is 6.8;
hue: the L value is 98.5%, the b value is 1.4, and the a value is 0.3;
the decolorization rate is 110 percent;
the dispersity is 7.0;
the water absorption capacity is 30g/50 g;
the oil absorption was 12g/100 g.
The results of the examples show that the titanium dioxide for the plastic color master batch provided by the invention has high whiteness, good dispersibility, good covering power and good oil absorption, and can meet the requirements of the plastic industry on the performance of the titanium dioxide.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (5)

1. Titanium white powder and TiO for plastic color master batch2The content of (a) is 95.5-98.5 wt%, wherein, the rutile type TiO2The content of (A) is more than or equal to 98.7 wt%; particle diameter D500.23 to 0.27 μm, particle diameter D99≤0.5μm；
Further comprises Al2O3Chlorotrimethylsilane, Fe2O3Said Al2O30.8-1.2 wt%, 0.7-1.0 wt% of trimethylchlorosilane, and Fe2O3The content of (A) is less than or equal to 0.005 wt%;
the preparation method of the titanium dioxide for the plastic color master batch comprises the following steps:
(1) adding ammonia water into the concentrated titanium solution until the pH value of the obtained mixed material is 2.4-2.6, heating the mixed material to 88-92 ℃ at the heating rate of 4.5-5.5 ℃/min, and preserving the heat for 4.5-5.5 min to obtain hydrolysis crystal seeds; wherein the process of adding ammonia water is controlled to be completed within 9-11 min;
(2) mixing the hydrolysis seed crystal in the step (1) with the concentrated titanium liquid at the temperature of 95-97 ℃, and hydrolyzing to obtain hydrolysis metatitanic acid slurry;
(3) washing the hydrolyzed metatitanic acid slurry obtained in the step (2) to obtain washed metatitanic acid slurry;
(4) adding calcined rutile type seed crystal, ZnO, and titanium dioxide into the washed metatitanic acid slurry obtained in the step (3) in sequence,NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Carrying out salt treatment to obtain salt-treated metatitanic acid slurry; the mass of the washing metatitanic acid slurry and the calcined rutile type seed crystal is TiO2Meter, NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3Respectively with the mass of P2O5、K2O、Al2O3And Ce2O3Washing metatitanic acid slurry, and calcining rutile type seed crystal, ZnO and NH4H2PO4KOH solution, Al2(SO4)3And Ce2(SO4)3The mass ratio of (A) to (B) is 100: (7-18): (0.10-0.16), (1-2), (1.3-2.5), (1-8): (0.05-0.10);
(5) filtering the salt-treated metatitanic acid slurry obtained in the step (4), and calcining the filtered solid material to obtain a crude product material;
(6) and (5) crushing and surface treating the crude product material in the step (5) to obtain the titanium dioxide for the plastic color master batch.
2. The titanium dioxide for plastic color masterbatch according to claim 1, wherein the content of 45 μm screen residue is not more than 0.01 wt%.
3. The titanium dioxide for plastic color masterbatch according to claim 1, wherein the specific surface area is 13-15 m2/g。
4. The titanium dioxide for plastic color masterbatch according to claim 1, wherein the volatile matter after drying for 2 hours at 105 ℃ is less than or equal to 0.2 wt%.
5. The titanium dioxide for plastic color masterbatch according to claim 1, wherein the drying is performed for 2 hours at 105 ℃, and the burning loss after burning for 1 hour at 900 ℃ is less than or equal to 0.3 wt%.
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CN106167275A (en) * 2016-08-03 2016-11-30 江苏大学 A kind of high whiteness high brightness technical grade rutile titanium dioxide former powder treatment preparation method thereof
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CN102325726A (en) * 2009-02-19 2012-01-18 堺化学工业株式会社 Dispersion of rutile titanium oxide particles, method for producing same and use of same
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