CN114539816A - Preparation method of special titanium dioxide for high-melting filterable color master batches - Google Patents
Preparation method of special titanium dioxide for high-melting filterable color master batches Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000004595 color masterbatch Substances 0.000 title claims abstract description 29
- 238000002844 melting Methods 0.000 title claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 35
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000002210 silicon-based material Substances 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000007865 diluting Methods 0.000 claims abstract description 3
- 239000012467 final product Substances 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 239000010703 silicon Substances 0.000 claims abstract description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 6
- 150000005846 sugar alcohols Polymers 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 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 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- 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 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 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 description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004061 bleaching Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 claims description 2
- 238000010902 jet-milling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000012756 surface treatment agent Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims 2
- 229930003427 Vitamin E Natural products 0.000 claims 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 229940046009 vitamin E Drugs 0.000 claims 1
- 235000019165 vitamin E Nutrition 0.000 claims 1
- 239000011709 vitamin E Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 19
- 230000001105 regulatory effect Effects 0.000 description 9
- 238000003825 pressing Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3669—Treatment with low-molecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3684—Treatment with organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Abstract
A preparation method of titanium dioxide powder special for high-melting filterability color master batches comprises the following steps: the method comprises the following steps: preparing titanium dioxide slurry; step two: silicon coating: diluting the titanium dioxide slurry obtained in the step one to the concentration of 300-450g/L, adding a dispersing agent, adjusting the pH, heating to the temperature of 60-80 ℃, and adding a silicon-containing compound to coat the surface of the titanium dioxide particles with a silicon oxide layer; step three: aluminum coating: adding an alumina compound into the slurry obtained in the second step, and measuring a hydrous alumina layer on the surface of the silica layer after hydrolysis; step four: and (3) drying: washing the titanium dioxide slurry obtained in the step three with water, filtering to obtain a filter cake, and drying; step five: and (4) crushing to obtain a final product. The titanium dioxide prepared by the invention has the advantages of good dispersibility, stable plastic melt filtration performance and the like, effectively overcomes the defects of poor dispersibility, unstable melt filtration pressure and the like of the titanium dioxide in the color master batch production process, and has simple preparation process and convenient wide popularization and use.
Description
Technical Field
The invention belongs to the field of titanium dioxide preparation, and particularly relates to a preparation method of titanium dioxide special for high-melting filterable color master batches.
Background
At present, the master batch titanium dioxide adopted in the titanium dioxide industry is mostly a general product, although the production of common master batches can be met, the problems of high-end master batches are solved, such as poor weather resistance, poor dispersibility, insufficient covering power, unstable filter pressing performance and the like.
Disclosure of Invention
The invention provides a preparation method of titanium dioxide special for high-melting filterable color master batches, which is used for overcoming the defects in the prior art.
The invention is realized by the following technical scheme:
a preparation method of titanium dioxide powder special for high-melting filterability color master batches comprises the following steps:
the method comprises the following steps: preparing titanium dioxide slurry: heating the titanium liquid added with the seed crystal and maintaining pressure for hydrolysis, preparing metatitanic acid by boiling twice, washing, bleaching and salting the metatitanic acid, squeezing the metatitanic acid into a filter cake, crushing the filter cake and calcining at the temperature of more than 950 ℃ to obtain a titanium dioxide crude product with the rutile content of more than or equal to 99.0 percent, crushing the titanium dioxide crude product, adding a dispersing agent, pulping and sanding the crushed titanium dioxide crude product to obtain titanium dioxide slurry with the particle size of less than 0.8 mu m;
step two: silicon coating: diluting the titanium dioxide slurry obtained in the step one to the concentration of 300-450g/L, adding a dispersing agent, adjusting the pH value of the slurry to 8-10, introducing steam, heating to 60-80 ℃, adding a silicon-containing compound while stirring, and maintaining the pH value of the slurry within the range of 8-9.5 so as to coat the surface of the titanium dioxide particles with a silicon oxide layer;
step three: aluminum coating: adding an alumina compound into the slurry obtained in the second step at the temperature of 50-60 ℃, measuring a hydrous alumina layer on the surface of the silica layer after hydrolysis, and maintaining the pH of the slurry within the range of 4-6 in the hydrolysis process;
step four: and (3) drying: washing the titanium dioxide slurry obtained in the step three with water, removing soluble salts by washing, filtering to obtain a filter cake, and drying at the temperature of 300-400 ℃;
step five: crushing: and D, primarily crushing the titanium dioxide obtained in the step four, then performing jet milling, and simultaneously adding an organic surface treating agent to obtain a final product.
In the preparation method of the titanium dioxide special for the high-melting filterability color master batch, the dispersant in the first step is any one or a mixture of any two or more of sodium hexametaphosphate, sodium silicate and sodium hydroxide mixed in any proportion.
According to the preparation method of the titanium dioxide powder special for the high-melting filterable color master batch, the addition amount of the dispersing agent in the first step is 0.01-0.2% of the mass of the titanium dioxide.
In the preparation method of the titanium dioxide powder special for the high-melting filterable color master batch, the dispersant in the second step is any one of a sodium dihydrogen phosphate solution and a sodium hexametaphosphate solution or a mixture of any two or more of the two in any proportion.
According to the preparation method of the titanium dioxide special for the high-melting filterable color master batches, the dispersant in the second step accounts for 0.01-0.2% of the mass of the titanium dioxide in terms of phosphorus pentoxide, and the concentration is 45-55 g/L.
According to the preparation method of the titanium dioxide special for the high-melting filterability color master batch, the silicon-containing compound in the second step is sodium silicate, and the sodium silicate is added into the titanium dioxide slurry in the form of aqueous solution.
According to the preparation method of the titanium dioxide special for the high-melting filterability color master batches, the sodium silicate accounts for 0.1-0.2% of the mass of the titanium dioxide in terms of the amount of the silicon oxide, and the concentration is 97-105 g/L.
In the preparation method of the titanium dioxide special for the high-melting filterable color master batch, the aluminum-containing compound in the third step is any one of sodium metaaluminate, aluminum sulfate, aluminum chloride and aluminum nitrate.
According to the preparation method of the titanium dioxide special for the high-melting filterable color master batch, the aluminum-containing compound in the third step is converted into aluminum oxide with the mass being 1.0-3.5% of that of titanium dioxide, and the concentration is 97-105 g/L.
According to the preparation method of the titanium dioxide special for the high-melting filterability color master batch, the resistivity of the filter cake obtained in the fourth step is more than or equal to 100 omega.M.
In the preparation method of the titanium dioxide special for the high-melting filterability color master batch, in the fifth step, any one of the organic surface treatment agent, namely the vitamin-silane coupling agent and the polyhydric alcohol is used.
According to the preparation method of the titanium dioxide special for the high-melting filterability color master batch, the adding amount of the organic surface treating agent is 0.1-1.0% of the mass of the titanium dioxide.
The invention has the advantages that: the titanium dioxide prepared by the invention has the advantages of good dispersibility, stable plastic melt filtration performance and the like, effectively overcomes the defects of poor dispersibility, unstable melt filtration pressure and the like of the titanium dioxide in the color master batch production process, can meet the production requirements of high-end color master batches, and has simple preparation process and convenient wide popularization and use.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a graph comparing the filtration pressure of examples 1-4 of the present invention with LR108, SR240, ATR312, R-104 prior art products;
FIG. 2 is a filter press test of example 1 of the present invention;
FIG. 3 is a filter press test of example 2 of the present invention;
FIG. 4 is a test of the filter pressing value of example 3 of the present invention;
FIG. 5 is a filter press test of example 4 of the present invention;
FIG. 6 is a filter-pressing value test of LR108, a prior domestic product;
FIG. 7 is a filter-pressing value test of the existing domestic product SR 240;
FIG. 8 is a filter press value test of the existing domestic product ATR 312;
FIG. 9 is a filter-press value test of R-104 of the existing foreign product.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present 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
With TiO2The method comprises the steps of regulating the concentration of slurry to 300g/L, regulating the adding amount of a dispersing agent to be 0.01%, regulating the pH value to be about 9.0, introducing steam to heat the slurry to 80 ℃, adding 0.1% of sodium silicate, fully dispersing and coating, cooling the temperature of the slurry to 60 ℃, adding 2.0% of an aluminum-containing compound, fully dispersing and coating, washing, squeezing and drying, and adding 0.4% of polyhydric alcohol in the process of steam powder to complete product preparation.
Example 2
With TiO2The concentration of the slurry is adjusted to 350g/L, the adding amount of the dispersing agent is 0.05 percent, the pH is adjusted to about 9.5, then steam is introduced to heat the slurry to 70 ℃, 0.1 percent of sodium silicate is added, and the slurry is fully dispersed and coatedCooling the slurry to 50 ℃, adding 1.0% of aluminum-containing compound, fully dispersing and coating, washing, squeezing and drying, and adding 0.5% of polyhydric alcohol in the process of steam powder to complete the preparation of the product.
Example 3
With TiO2The method comprises the steps of regulating the concentration of slurry to 400g/L, regulating the addition amount of a dispersing agent to 0.1%, regulating the pH value to about 10, introducing steam to heat the slurry to 60 ℃, adding 0.15% of sodium silicate, fully dispersing and coating, cooling the temperature of the slurry to 60 ℃, adding 2.5% of an aluminum-containing compound, fully dispersing and coating, washing with water, squeezing, drying, and adding 0.7% of a silane coupling agent in the process of steam powder to complete product preparation.
Example 4
With TiO2The method comprises the steps of regulating the concentration of slurry to 450g/L, regulating the adding amount of a dispersing agent to be 0.2%, regulating the pH value to be about 9.0, introducing steam to heat the slurry to 70 ℃, adding 0.2% of sodium silicate, fully dispersing and coating, cooling the temperature of the slurry to 60 ℃, adding 3.5% of an aluminum-containing compound, fully dispersing and coating, washing, squeezing and drying, and adding 1.0% of polyhydric alcohol in the process of steam powder to complete product preparation.
The products prepared in the examples 1 to 4 and the existing products LR108, SR240, ATR312 and R-104 are subjected to pressure test, the LR108, SR240 and ATR312 are special products for domestic color master batches, the R-104 is a special product for foreign color master batches, and the results are shown in the table I.
Watch 1
As can be seen from the table I and the figures 1 to 8, the starting pressure and the maximum pressure of the production of the invention in the implementation 1 to 4 are all less than those of domestic products LR108, SR240 and ATR312, so that the titanium dioxide prepared by the invention is proved to have good filtration stability, and although the performance of the product prepared by the invention in the implementation 1 to 4 is slightly poor compared with that of a foreign product R-104, the preparation cost of the invention is obviously reduced compared with that of the product R-104, and the performance difference is only slightly poor, but the selling price of the invention is reduced by 30 to 40 percent compared with that of the product R-104, thereby being convenient for wide popularization and use.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A preparation method of titanium dioxide special for high-melting filterability color master batches is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparing titanium dioxide slurry: heating the titanium liquid added with the seed crystal and maintaining pressure for hydrolysis, preparing metatitanic acid by boiling twice, washing, bleaching and salting the metatitanic acid, squeezing the metatitanic acid into a filter cake, crushing the filter cake and calcining at the temperature of more than 950 ℃ to obtain a titanium dioxide crude product with the rutile content of more than or equal to 99.0 percent, crushing the titanium dioxide crude product, adding a dispersing agent, pulping and sanding the crushed titanium dioxide crude product to obtain titanium dioxide slurry with the particle size of less than 0.8 mu m;
step two: silicon coating: diluting the titanium dioxide slurry obtained in the step one to the concentration of 300-450g/L, adding a dispersing agent, adjusting the pH value of the slurry to 8-10, introducing steam, heating to 60-80 ℃, adding a silicon-containing compound while stirring, and maintaining the pH value of the slurry within the range of 8-9.5 so as to coat the surface of the titanium dioxide particles with a silicon oxide layer;
step three: aluminum coating: adding an alumina compound into the slurry obtained in the second step at the temperature of 50-60 ℃, measuring a hydrous alumina layer on the surface of the silica layer after hydrolysis, and maintaining the pH of the slurry within the range of 4-6 in the hydrolysis process;
step four: and (3) drying: washing the titanium dioxide slurry obtained in the step three with water, removing soluble salts by washing, filtering to obtain a filter cake, and drying at the temperature of 300-400 ℃;
step five: crushing: and D, primarily crushing the titanium dioxide obtained in the step four, then performing jet milling, and simultaneously adding an organic surface treating agent to obtain a final product.
2. The preparation method of the titanium dioxide powder with high melting and filtering properties special for the color master batch according to claim 1, which is characterized in that:
the dispersant in the first step is any one or a mixture of any two or more of sodium hexametaphosphate, sodium silicate and sodium hydroxide which are mixed in any proportion;
the addition amount of the dispersing agent in the first step is 0.01-0.2% of the mass of the titanium dioxide.
3. The preparation method of the titanium dioxide powder special for the high-melting filterability color master batch according to the patent claim 1 is characterized by comprising the following steps:
the dispersant in the second step is any one or a mixture of any two or more of a sodium dihydrogen phosphate solution and a sodium hexametaphosphate solution which are mixed in any proportion;
and in the second step, the dispersant accounts for 0.01 to 0.2 percent of the mass of the titanium dioxide in terms of phosphorus pentoxide, and the concentration is 45 to 55 g/L.
4. The preparation method of the titanium dioxide powder special for the high-melting filterability color master batch according to claim 1, characterized by comprising the following steps:
the silicon-containing compound in the second step is sodium silicate and is added into the titanium dioxide slurry in the form of aqueous solution;
the sodium silicate is 0.1-0.2% of the titanium dioxide by weight based on the silica content, and the concentration is 97-105 g/L.
5. The preparation method of the titanium dioxide powder special for the high-melting filterability color master batch according to claim 1, characterized by comprising the following steps:
the aluminum-containing compound in the third step is any one of sodium metaaluminate, aluminum sulfate, aluminum chloride and aluminum nitrate;
the aluminum-containing compound in the third step is converted into aluminum oxide with the mass being 1.0-3.5% of that of the titanium dioxide, and the concentration is 97-105 g/L.
6. The preparation method of the titanium dioxide powder special for the high-melting filterability color master batch according to claim 1, characterized by comprising the following steps: and the resistivity of the filter cake obtained in the fourth step is more than or equal to 100 omega.M.
7. The preparation method of the titanium dioxide powder special for the high-melting filterability color master batch according to claim 1, characterized by comprising the following steps:
any one of the organic surface treating agent, namely the vitamin E silane coupling agent and the polyhydric alcohol in the step five;
the addition amount of the organic surface treatment agent is 0.1-1.0% of the mass of the titanium dioxide.
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