CN117285829A - Titanium dioxide surface treatment process - Google Patents
Titanium dioxide surface treatment process Download PDFInfo
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- CN117285829A CN117285829A CN202310976987.XA CN202310976987A CN117285829A CN 117285829 A CN117285829 A CN 117285829A CN 202310976987 A CN202310976987 A CN 202310976987A CN 117285829 A CN117285829 A CN 117285829A
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- titanium dioxide
- sodium
- sodium metaaluminate
- treatment process
- surface treatment
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004381 surface treatment Methods 0.000 title claims abstract description 23
- 239000011734 sodium Substances 0.000 claims abstract description 64
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 59
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 59
- 239000002002 slurry Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 238000004537 pulping Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000011282 treatment Methods 0.000 claims description 2
- 239000001038 titanium pigment Substances 0.000 claims 8
- 238000002156 mixing Methods 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 14
- 238000000576 coating method Methods 0.000 abstract description 14
- 239000006185 dispersion Substances 0.000 abstract description 5
- 230000002708 enhancing effect Effects 0.000 abstract description 4
- 235000010215 titanium dioxide Nutrition 0.000 description 61
- 230000001276 controlling effect Effects 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011573 trace mineral Substances 0.000 description 3
- 235000013619 trace mineral Nutrition 0.000 description 3
- QDYLZPZHGWKOBI-UHFFFAOYSA-N [AlH3].[Na].[Na] Chemical compound [AlH3].[Na].[Na] QDYLZPZHGWKOBI-UHFFFAOYSA-N 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/3623—Grinding
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/363—Drying, calcination
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
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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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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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Abstract
The invention provides a titanium dioxide surface treatment process, which comprises the following steps: (1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry; (2) Heating titanium dioxide slurry to raise the temperature, and adding a dispersing agent in the heating process; after the temperature is raised, adding zirconium sulfate, and controlling the pH value to be 1.8-2.3; (3) Then sequentially adding sodium metaaluminate solution and aluminum sulfate at least once, wherein the sodium metaaluminate is prepared by reacting amphoteric aluminum hydroxide with excessive alkali, and controlling the sodium-aluminum ratio to be 1.3-1.6; (4) Washing and press-filtering the materials to obtain a filter cake, and performing a flash dry gas powder procedure to obtain finished titanium dioxide; the dispersion state of the inorganic coating of the titanium dioxide can be improved, and the aims of reducing consumption and enhancing efficiency are fulfilled.
Description
Technical Field
The invention relates to the technical field of titanium dioxide processing, in particular to a titanium dioxide surface treatment process.
Background
Titanium dioxide (commonly called titanium dioxide) is the best white pigment in the world at present, has very stable physical and chemical properties, and also has excellent optical and electrical properties such as high refractive index, optimal hiding power, optimal whiteness, brightness and the like, and is widely applied to the fields of paint, plastics, papermaking, printing ink, electronics and the like. In the paper making field, the decorative paper is one of the most titanium dioxide, the quality of the decorative paper using titanium dioxide is high, especially white decorative paper, and the using amount of the titanium dioxide can reach 45%. The decorative paper is a component part of a coating material of decorative thermosetting plastic, is placed below surface paper in a product structure, and the surface of the decorative paper is not required to be coated after being pressed, so that the decorative paper mainly has the decorative effect of providing a pattern and the covering effect of preventing the glue solution of the bottom layer from seeping. The titanium dioxide for the decorative paper should have good hiding power, weather resistance (chalking resistance), color fastness and water dispersibility so as to ensure that the decorative paper has excellent service performance. However, some photo-activation points exist on the surface of the titanium dioxide powder particles, so that the titanium dioxide pigment has a photo-catalytic effect, and under the irradiation of sunlight, particularly ultraviolet rays, a photo-catalytic reaction occurs, so that organic components in contact with the titanium dioxide are degraded and pulverized, and various performances and service lives of the decorative paper are seriously affected. Therefore, titanium dioxide pigments used for decorative papers often require special surface treatments.
In the prior art, titanium dioxide is generally subjected to inorganic surface treatment after beating and dispersing. The titanium dioxide is subjected to a certain amount of inorganic coating under a certain pH condition, so that the weather resistance, the dispersion performance and the like of the titanium dioxide are improved, however, when the titanium dioxide is subjected to surface treatment, more sodium salt is formed, the dispersibility and the viscosity of the slurry are affected, the uniformity of the coating is poor, and the whiteness, the weather resistance, the dispersibility and other application performance indexes of the product are reduced. The excess alkali exists in the form of sulfate, which not only increases the load of three washes, but also increases the cost of coating.
Disclosure of Invention
The invention aims to provide a titanium dioxide surface treatment process which can improve the dispersion state of an inorganic coating of titanium dioxide and achieve the aims of reducing consumption and enhancing efficiency.
The embodiment of the invention is realized by the following technical scheme:
preparation of high concentration sodium metaaluminate solution
Adopts an aluminum hydroxide alkaline hydrolysis method, namely, amphoteric aluminum hydroxide reacts with excessive alkali to generate sodium metaaluminate. I.e. according to the sodium-aluminum ratio of 1.3-1.6 (or Na 2 190-210g/L O) to prepare a mixed solution of aluminum hydroxide and sodium hydroxide (50%), stirring, heating by steam to 110-120 ℃, keeping boiling for 180-240min, and adding water to dilute to Al 2 O 3 The concentration is 195-205g/L, hydrogen280-320g/L of sodium oxide.
The preparation process comprises the following steps: (at 17 m) 3 Reaction kettle, preparation 14m 3 High concentration sodium metaaluminate is taken as an example
Determining proper Na 2 O concentration (190-210 g/L, i.e. Na/Al ratio 1.3-1.6);
adding 1.5-2 m of bottom water (copper salt water) into the reaction kettle 2 The aim is to control the reaction basicity;
thirdly, adding 4.3 to 4.5t of solid aluminum hydroxide;
adding 50% sodium hydroxide solution;
fifthly, starting steam to heat to 110-120 ℃;
adjusting the steam size, keeping the reaction kettle in a micro-boiling state, controlling the temperature to be more than or equal to 105 ℃ and controlling the time to be 180-240min;
adding 3.5-4.5m of metered dilution water 3 ；
And cooling and removing impurities from the sodium metaaluminate solution by adopting a natural sedimentation cooling (60-65 ℃) mode and a filter press filtering mode and a screen filtering mode.
When the method is used for preparing the high-concentration sodium metaaluminate, the sodium-aluminum ratio of the sodium metaaluminate solution is reduced, the input cost is considered, and the stability of the high-concentration sodium metaaluminate (without hydrolysis or crystallization) is ensured under the condition that other reagents are not added; and impurity removal control is carried out in a filtering crystallization sucking mode to prepare sodium metaaluminate, so that the cleanliness of the sodium metaaluminate is ensured.
A titanium dioxide surface treatment process comprises the following steps:
(1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry, and controlling TiO in the slurry 2 The concentration is 500-600g/L, the pH value is 9.4-10, and the particle diameter D50:0.32-0.38um;
(2) Adjusting the concentration and PH value of the titanium dioxide slurry, and controlling TiO 2 The content of (C) is 280-320g/l and the pH value is 9-10.5. And simultaneously, starting steam heating, and controlling the temperature to be 60+/-5 ℃. Adding dispersant sodium hexametaphosphate in the heating process, wherein the adding amount is 0.9-1.2 kg/ton TiO 2 Counting; after the temperature is raised, 0.23 to 0.26 percent of zirconium sulfate (the adding amount is titanium white)The weight percentage of titanium dioxide contained in the slurry is calculated as follows, the adding time is 40min, stirring is carried out for 30min, and the pH value is controlled to be 1.8-2.3;
(3) Then adding the prepared sodium metaaluminate (the content of the sodium metaaluminate is 195-205g/L, the content of the sodium hydroxide is 280-320 g/L), the adding speed of the sodium metaaluminate is 45-60L/min according to different adding amounts of products, the adding time is 30-140min, the temperature is controlled to be 55-60 ℃ after adding, and the stirring is carried out for 45min, and the PH value is 9.0-9.5;
(4) Adding 0.8-1.0% aluminum sulfate for 50min, stirring for 30min, and controlling pH at 2.8-3.5;
(6) Adding 1.65-1.85% sodium metaaluminate for 120min, stirring for 60min, and controlling pH at 9.5-10.3;
(7) Adding a small amount of aluminum sulfate to adjust the pH value to 7.4-7.8, and curing for 120min;
(8) And after the coating is finished, washing and press-filtering the materials to obtain a filter cake, and then performing a flash dry gas powder process to obtain the finished titanium dioxide.
The invention reduces the sodium-aluminum ratio of the sodium metaaluminate solution to the coated titanium dioxide, reduces the alkali consumption and improves the Al 2 O 3 Concentration; improving the dispersion state of the inorganic coating and achieving the aims of reducing consumption and enhancing efficiency.
The technical scheme of the embodiment of the invention has at least the following advantages and beneficial effects:
1. when the method is used for preparing the high-concentration sodium metaaluminate, the sodium-aluminum ratio of the sodium metaaluminate solution is reduced, the input cost is considered, and the stability of the high-concentration sodium metaaluminate (without hydrolysis or crystallization) is ensured under the condition that other reagents are not added; and impurity removal control is carried out in a filtering crystallization sucking mode to prepare sodium metaaluminate, so that the cleanliness of the sodium metaaluminate is ensured.
2. The invention reduces the sodium-aluminum ratio of the sodium metaaluminate solution to the coated titanium dioxide, reduces the alkali consumption and improves the Al 2 O 3 Concentration; improving the dispersion state of the inorganic coating, improving the uniformity of the coating, the whiteness and the weather resistance of the product, and achieving the aims of reducing consumption and enhancing efficiency.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
1. Preparation of high concentration sodium metaaluminate solution
Preparing a mixed solution of aluminum hydroxide and sodium hydroxide (50%) according to a sodium-aluminum ratio of 1.5, adding bottom water, stirring, heating with steam to 115 ℃, keeping boiling for 200min, and diluting with water to Al 2 O 3 Concentration is 200g/L, and sodium hydroxide is 300g/L; and finally, naturally settling and cooling the sodium metaaluminate solution to 63 ℃, filtering, and sucking out crystals to obtain sodium metaaluminate.
2. The titanium dioxide surface treatment process comprises the following steps:
(1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry, and controlling TiO in the slurry 2 Concentration 550g/L, pH 9.7, particle size D50:0.35um;
(2) Adjusting the concentration and PH value of the titanium dioxide slurry, and controlling TiO 2 The content of (C) is 300g/l and the pH value is 9.5; and simultaneously, steam heating is started, and the temperature is controlled to be 60 ℃. Adding dispersant sodium hexametaphosphate in the heating process according to the addition amount of 1.0 kg/ton TiO 2 Counting; after the temperature is raised, adding 0.25% of zirconium sulfate (the addition amount is calculated by the weight percentage of titanium dioxide contained in the titanium dioxide slurry, the same applies below), adding for 40min, stirring for 30min, and controlling the pH value to be 2.0;
(3) Then adding the prepared sodium metaaluminate, wherein the addition amount of the sodium metaaluminate is 2 percent of the weight of titanium dioxide contained in the titanium dioxide slurry, the adding speed of the sodium metaaluminate is 50L/min, the adding time is 100min, the temperature is controlled to be 58 ℃ after the adding, and the stirring is carried out for 45min, and the PH value is 9.3;
(4) Adding 1% aluminum sulfate for 50min, stirring for 30min, and controlling pH value at 3;
(6) Adding 1.7% sodium metaaluminate for 120min, stirring for 60min, and controlling pH value at 10;
(7) Adding a small amount of aluminum sulfate to adjust the pH value to 7.6, and curing for 120min;
(8) And after the coating is finished, washing and press-filtering the materials to obtain a filter cake, and then performing a flash dry gas powder process to obtain the finished titanium dioxide.
The surface treatment was carried out at 25 tons/batch, and the sodium aluminum sodium metaaluminate ratio was reduced, and then the NaOH (100% by weight) was added at 373Kg.
Example 2
1. Preparation of high concentration sodium metaaluminate solution
Preparing a mixed solution of aluminum hydroxide and sodium hydroxide (50%) according to a sodium-aluminum ratio of 1.3, adding bottom water, stirring, heating with steam to 110 ℃, keeping boiling for 180min, and diluting with water to Al 2 O 3 The concentration is 195g/L, and the concentration of sodium hydroxide is 280g/L; and finally, naturally settling and cooling the sodium metaaluminate solution to 60 ℃, filtering, and sucking out crystals to obtain sodium metaaluminate.
2. The titanium dioxide surface treatment process comprises the following steps:
(1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry, and controlling TiO in the slurry 2 Concentration 500g/L, pH 9.4, particle size D50:0.32um;
(2) Adjusting the concentration and PH value of the titanium dioxide slurry, and controlling TiO 2 The content of (C) is 280g/l and the pH value is 9; and simultaneously, starting steam heating, and controlling the temperature to be 55 ℃. Adding dispersant sodium hexametaphosphate in the heating process according to the addition amount of 0.9 kg/ton TiO 2 Counting; after the temperature is raised, adding 0.23% of zirconium sulfate (the addition amount is calculated by the weight percentage of titanium dioxide contained in the titanium dioxide slurry, the same applies below), adding for 40min, stirring for 30min, and controlling the pH value to be 1.8;
(3) Then adding the prepared sodium metaaluminate, wherein the addition amount of the sodium metaaluminate is 0.88 percent of the weight of titanium dioxide contained in the titanium dioxide slurry, the adding speed of the sodium metaaluminate is 45L/min, the adding time is 30min, the temperature is controlled to be 55 ℃ after the adding, and the stirring is carried out for 45min, and the PH value is 9.0;
(4) Adding 0.9% aluminum sulfate for 50min, stirring for 30min, and controlling pH value at 2.8;
(6) Adding 1.75% sodium metaaluminate for 120min, stirring for 60min, and controlling pH value at 9.5-10.3;
(7) Adding a small amount of aluminum sulfate to adjust the pH value to 7.4, and curing for 120min;
(8) And after the coating is finished, washing and press-filtering the materials to obtain a filter cake, and then performing a flash dry gas powder process to obtain the finished titanium dioxide.
The surface treatment was carried out in a 25 ton/batch, and the addition of NaOH (100%) was reduced to 199Kg after the sodium aluminum sodium meta-aluminate ratio was reduced.
Example 3
1. Preparation of high concentration sodium metaaluminate solution
Preparing a mixed solution of aluminum hydroxide and sodium hydroxide (50%) according to a sodium-aluminum ratio of 1.6, adding bottom water, stirring, heating with steam to 120 ℃, keeping boiling for 240min, and adding water to dilute to Al 2 O 3 Concentration 205g/L, sodium hydroxide 320g/L; and finally, naturally settling and cooling the sodium metaaluminate solution to 65 ℃, filtering, and sucking out crystals to obtain sodium metaaluminate.
2. The titanium dioxide surface treatment process comprises the following steps:
(1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry, and controlling TiO in the slurry 2 Concentration 600g/L, pH 10, particle size D50:0.38um;
(2) Adjusting the concentration and PH value of the titanium dioxide slurry, and controlling TiO 2 The content of (C) is 320g/l and the pH value is 10.5; and simultaneously, starting steam heating, and controlling the temperature to be 65 ℃. Adding dispersant sodium hexametaphosphate in the heating process, wherein the adding amount is 1.2 kg/ton TiO 2 Counting; after the temperature is raised, adding 0.26% of zirconium sulfate (the addition amount is calculated by the weight percentage of titanium dioxide contained in the titanium dioxide slurry, the same applies below), adding for 40min, stirring for 30min, and controlling the pH value to be 2.3;
(3) Then adding the prepared sodium metaaluminate, wherein the addition amount of the sodium metaaluminate is 4 percent of the weight of titanium dioxide contained in the titanium dioxide slurry, the adding speed of the sodium metaaluminate is 60L/min, the adding time is 140min, the temperature is controlled to be 60 ℃ after the adding, and the stirring is carried out for 45min, and the PH value is 9.5;
(4) Adding 0.95% aluminum sulfate for 50min, stirring for 30min, and controlling pH value at 3;
(6) Adding 1.7% sodium metaaluminate for 120min, stirring for 60min, and controlling pH value at 10;
(7) Adding a small amount of aluminum sulfate to adjust the pH value to 7.8, and curing for 120min;
(8) And after the coating is finished, washing and press-filtering the materials to obtain a filter cake, and then performing a flash dry gas powder process to obtain the finished titanium dioxide.
The surface treatment was carried out at a rate of 25 tons/batch, and after the sodium aluminum meta-aluminate ratio was reduced, the addition of NaOH (100% was reduced) was 699Kg.
Comparative example 1
This comparative example differs from example 1 in that: the sodium-aluminum ratio when preparing the high-concentration sodium metaaluminate solution is 2.5.
Comparative example 2
This comparative example differs from example 1 in that: the sodium-aluminum ratio when preparing the high-concentration sodium metaaluminate solution is 1.0.
Experimental example 1
The whiteness and brightness values of the products of the examples and the comparative examples are measured by using a color difference meter, and the results are shown in Table 1:
table 1: whiteness and brightness values of the products
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| L | 100.9 | 101.0 | 100.6 | 98.1 | 100.3 |
| a | 0.04 | 0.05 | 0.07 | -0.01 | -0.02 |
| b | 1.20 | 1.23 | 1.25 | 1.32 | 1.30 |
Where "L" represents the brightness of the object, "a" represents the red-green color of the object, and "b" represents the yellow-blue color of the object.
As can be seen from table 1, the whiteness of the titanium dioxide after treatment is normal, and the brightness value is obviously increased; the ratio of sodium to aluminum is not in the range of the invention, namely, the ratio of sodium to aluminum is too high or too low, the whiteness of the titanium white is reduced, and the brightness is darker.
Experimental example 2
The trace elements (%) in each group of titanium dioxide were analyzed as follows:
table 2: trace element results in each group of titanium dioxide
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| TiO 2 | 92.3971 | 93.4157 | 93.6345 | 85.8052 | 80.2148 |
| Na | 0.0283 | 0.0303 | 0.0291 | 0.1125 | 0.0148 |
| Ca | 0.0061 | 0.0097 | 0.0086 | 0.0091 | 0.0021 |
| Fe | 0.0048 | 0.0041 | 0.0043 | 0.0035 | 0.0018 |
| Al 2 O 3 | 3.4476 | 3.2614 | 3.3155 | 5.2439 | 1.8957 |
| K 2 O | 0.0074 | 0.0115 | 0.0096 | 0.0981 | 0.0058 |
| P 2 O 5 | 0.2554 | 0.2567 | 0.21481 | 2.9419 | 0.1489 |
| SiO 2 | 0.0466 | 0.0482 | 0.0468 | 0.0475 | 0.0348 |
| ZnO | 0.0885 | 0.1023 | 0.0911 | 0.1045 | 0.0581 |
As can be seen from Table 2, the titanium white powder treated by the method has high aluminum coating rate and relatively low total trace element content, and particularly, sodium salt on the surface of the titanium white powder is reduced after the sodium-aluminum ratio is regulated, so that the dispersibility and viscosity of the slurry are greatly improved.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The titanium dioxide surface treatment process is characterized by comprising the following steps of:
(1) Crushing, pulping and sanding the crude titanium dioxide to obtain titanium dioxide slurry;
(2) Heating titanium dioxide slurry to raise the temperature, and adding a dispersing agent in the heating process; after the temperature is raised, adding zirconium sulfate, and controlling the pH value to be 1.8-2.3;
(3) Then sequentially adding sodium metaaluminate solution and aluminum sulfate at least once, wherein the sodium metaaluminate is prepared by reacting amphoteric aluminum hydroxide with excessive alkali, and controlling the sodium-aluminum ratio to be 1.3-1.6;
(4) Washing and press-filtering the material to obtain a filter cake, and then performing a flash dry gas powder procedure to obtain the finished titanium dioxide.
2. The titanium pigment surface treatment process according to claim 1, wherein the TiO in the slurry is controlled in step (1) 2 The concentration is 500-600g/L, the pH value is 9.4-10, and the particle diameter D50:0.32-0.38um.
3. The titanium dioxide surface of claim 1The treatment process is characterized in that the temperature is controlled to be 55-65 ℃ in the step (2); the addition amount of the dispersing agent is 0.9-1.2 kg/ton TiO 2 And (5) counting.
4. The titanium pigment surface treatment process according to claim 1, wherein the zirconium sulfate added in the step (2) is 0.23 to 0.26% by weight of the titanium dioxide contained in the titanium pigment slurry.
5. The titanium pigment surface treatment process according to claim 1, wherein the sodium metaaluminate content in the sodium metaaluminate solution in the step (3) is 195-205g/L, and the sodium hydroxide content is 280-320g/L.
6. The titanium pigment surface treatment process according to claim 1, wherein the adding speed of the sodium metaaluminate solution in the step (3) is 45-60L/min, and the adding time is 30-140min.
7. The titanium pigment surface treatment process according to claim 1, wherein in the step (3), when sodium metaaluminate solution and aluminum sulfate are added, the process comprises the following steps:
(3.1) adding sodium metaaluminate according to 0.18-4% of the weight of titanium dioxide contained in the titanium dioxide slurry, controlling the temperature to be 55-60 ℃ and the PH value to be 9.0-9.5;
(3.2) adding aluminum sulfate according to 0.8-1.0% of the weight of titanium dioxide in the titanium dioxide slurry, and controlling the pH value to be 2.8-3.5;
(3.3) adding sodium metaaluminate according to 1.65-1.85% of the weight of titanium dioxide contained in the titanium dioxide slurry, and controlling the pH value to be 9.5-10.3;
(3.4) finally adding a small amount of aluminum sulfate to adjust the pH value to 7.4-7.8, and curing for 120min.
8. The titanium pigment surface treatment process according to claim 1, wherein the preparation method of sodium metaaluminate in the step (3) comprises the following steps: according to the sodium-aluminum ratio of 1.3-1.6 or Na 2 Mixing with mixed solution of aluminum hydroxide and 50% sodium hydroxide, adding bottom water, stirring to obtain solution with O concentration of 190-210g/LStirring, heating to 110-120deg.C, boiling for 180-240min, and diluting with water to Al 2 O 3 The concentration is 195-205g/L, and the concentration of sodium hydroxide is 280-320g/L; and finally, naturally settling, cooling, filtering and crystallizing the sodium metaaluminate solution to obtain sodium metaaluminate.
9. The titanium pigment surface treatment process according to claim 8, wherein the sodium metaaluminate is prepared by natural sedimentation cooling to 60-65 ℃.
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