CN111320885A - Titanium dioxide special for color master batch and preparation method thereof - Google Patents
Titanium dioxide special for color master batch and preparation method thereof Download PDFInfo
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- CN111320885A CN111320885A CN201811529861.3A CN201811529861A CN111320885A CN 111320885 A CN111320885 A CN 111320885A CN 201811529861 A CN201811529861 A CN 201811529861A CN 111320885 A CN111320885 A CN 111320885A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 205
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 82
- 239000004595 color masterbatch Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 37
- 239000011248 coating agent Substances 0.000 claims abstract description 32
- 238000000576 coating method Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000008394 flocculating agent Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 51
- 239000000843 powder Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 10
- 239000013067 intermediate product Substances 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000011362 coarse particle Substances 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920000142 Sodium polycarboxylate Polymers 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000009837 dry grinding Methods 0.000 claims description 4
- 238000004537 pulping Methods 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 125000005375 organosiloxane group Chemical group 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005189 flocculation Methods 0.000 abstract description 5
- 230000016615 flocculation Effects 0.000 abstract description 5
- 238000004381 surface treatment Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001694 spray drying Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 24
- 239000000047 product Substances 0.000 description 8
- 239000012065 filter cake Substances 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- -1 polydimethylsiloxane Polymers 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000012463 white pigment Substances 0.000 description 3
- 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 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 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 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 241001399594 Venator Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
-
- 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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09C3/10—Treatment with macromolecular organic compounds
-
- 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
- C09C3/12—Treatment with organosilicon compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention relates to a titanium dioxide special for color master batch and a preparation method thereof, wherein titanium dioxide particles of the titanium dioxide special for the color master batch are rutile type titanium dioxide particles; the surface of the rutile type titanium dioxide particles is coated with an organic coating, and is not coated with an aluminum coating. In the preparation method, the flocculating agent is adopted to replace an inorganic aluminum coating to achieve the flocculation effect, or the spray drying is adopted to save the inorganic coating flocculation step. The inorganic surface treatment process in the traditional titanium dioxide post-treatment process is omitted, the process flow is short, the production cost is low, and the product has high dispersibility, strong covering power and low water content.
Description
Technical Field
The invention relates to titanium dioxide special for color master batches and a preparation method thereof, belonging to the technical field of titanium dioxide production by a sulfuric acid method.
Background
Titanium dioxide (TiO)2) The white pigment has stable physical and chemical properties, high opacity, high whiteness and high brightness, is a white pigment with optimal performance, and is widely applied to the industries of coatings, plastics, printing ink, papermaking and the like. The plastic is the second field of application of titanium dioxide, and the titanium dioxide is used as a white pigment with the best performance, so that high whiteness and high covering power can be provided for the plastic, the heat resistance, weather resistance and processability of a plastic product can be improved, and the service life of the plastic is prolonged. The color master batch is a plastic colorant prepared by well dispersing a pigment or an additive and a thermoplastic resin with a high proportion, and the titanium dioxide content of the high-concentration color master batch can reach 60-80%. The titanium dioxide special for the color master batch is required to have good dispersibility and covering power. Meanwhile, the special titanium dioxide for the color master batch also requires low water content, so that the phenomenon of film foaming of the color master batch is prevented when the color master batch is used.
At present, in order to improve the dispersibility of the special titanium dioxide for the color master batch, an inorganic surface treatment process is required in the production process, and the inorganic surface treatment process is mainly an inorganic aluminum coating. For example, CN101891973A discloses a titanium dioxide pigment special for color master batches and a preparation method thereof, wherein the scheme comprises an aluminum coating step, the preparation method is long in time, requires 6-8 hours, restricts production, has low dispersibility, and cannot meet the requirement of the titanium dioxide special for the color master batches on high dispersibility. CN104194409A discloses a preparation method and application of high-temperature-resistant titanium dioxide by a mechanism, wherein the patent adopts a coating process of coating a layer of aluminum phosphate film on the surface of titanium dioxide and then coating a layer of aluminum oxide film, the coating process is complex, and the condition is difficult to control. CN102516824A and CN103013184A respectively disclose a preparation method of special titanium dioxide for color master batches, and the aluminum content is more than 1 percent.
Disclosure of Invention
In order to solve the problems, the invention provides special titanium dioxide for color master batches, which has good dispersibility and low water content and specifically comprises the following components:
the special titanium dioxide for the color master batch comprises titanium dioxide particles, wherein the titanium dioxide particles are rutile type titanium dioxide particles; the surface of the rutile type titanium dioxide particles is coated with an organic coating, and is not coated with an aluminum coating.
Further, the organic coating is one or a mixture of silane coupling agent, organic siloxane, silicone oil and organic phosphoric acid.
The invention also provides a preparation method of the special titanium dioxide for the color master batch, which comprises the following steps:
(1) dry grinding the sulfuric acid process rutile type titanium dioxide crude product to ensure that the particle size of 95 percent of titanium dioxide particles is less than 10 microns;
(2) pulping the titanium dioxide ground by the dry method to obtain TiO2Adding sodium polycarboxylate serving as a dispersing agent into slurry with the concentration of 700 g/L-800 g/L, depolymerizing titanium dioxide coarse particles in the slurry through three-stage sanding, and further removing the large particles from the sanded slurry through a cyclone to obtain sanded slurry;
(3) adding a flocculating agent into the sand grinding slurry obtained in the step (2) to flocculate titanium dioxide particles in the slurry, filtering and washing the flocculated slurry, and drying the slurry by using a flash evaporator to obtain a titanium dioxide intermediate product;
(4) performing steam flow crushing on the titanium dioxide intermediate product obtained in the step (3), and adding an organic coating agent to obtain titanium dioxide special for color master batches; wherein the addition amount of the organic coating agent is TiO20.3-0.8% of the mass.
Further, in the step (3), the added flocculating agent is an organic flocculating agent, and the adding amount of the flocculating agent is TiO20.01 to 0.1% by mass.
Further, the organic flocculant is a polyacrylamide flocculant.
The other preparation method of the special titanium dioxide for the color master batch comprises the following steps:
(1) dry grinding the sulfuric acid process rutile type titanium dioxide crude product to ensure that the particle size of 95 percent of titanium dioxide particles is less than 10 microns;
(2) pulping the titanium dioxide ground by the dry method to obtain TiO2Adding sodium polycarboxylate serving as a dispersing agent into slurry with the concentration of 700-800 g/L, depolymerizing coarse titanium dioxide particles in the slurry through three-stage sanding, and sandingThe large particles of the rear slurry are further removed through a cyclone to obtain sanding slurry;
(3) directly feeding the sand grinding slurry obtained in the step (2) into a centrifugal spray dryer for drying to obtain a titanium dioxide intermediate product;
(4) performing steam flow crushing on the titanium dioxide intermediate product obtained in the step (3), and adding an organic coating agent to obtain titanium dioxide special for color master batches; wherein the addition amount of the organic coating agent is TiO20.3-0.8% of the mass.
Further, in the step (2), TiO2After sanding, the particle size D50 of the crude product is controlled to be 0.2-0.22 μm, and the particle size distribution coefficient PSD is controlled to be 0.7-0.9.
Further, in the step (4), the organic coating agent is one or a mixture of more of a silane coupling agent, organic siloxane, silicone oil and organic phosphoric acid.
In the production process of titanium dioxide, the dispersibility of titanium dioxide particles can be improved by inorganic aluminum coating treatment. The inventor finds that the actual effect of inorganic aluminum coating by using the titanium dioxide special for the color master batch is to flocculate and precipitate the sand grinding slurry, facilitate three times of washing and then dry a filter cake. But the inorganic aluminum coating process has long coating time, so that the yield is reduced and the production cost is increased. The inorganic aluminum coating can generate flocculation coarse particles which are difficult to disperse, and further influences the product dispersibility. And the inorganic aluminum can bring crystal water, so that the color master batch can generate a foaming phenomenon in use.
The main innovation point of the application is that the flocculating agent is adopted to replace an inorganic aluminum coating to achieve the effect of flocculation, or the step of inorganic coating flocculation is omitted by adopting spray drying. Its main advantage is: the inorganic surface treatment process in the traditional titanium dioxide post-treatment process is omitted, the process flow is short, the production cost is low, the product dispersibility is high, the covering power is strong, the water content is low, and the special titanium dioxide level of the international excellent color master batch is reached.
Detailed Description
Example 1
a. Preparation of TiO2Slurry preparation: calcining TiO in a rotary kiln2Crude product JingleiThe concentration (prepared by TiO) is obtained after the Mongolian grinding dry method dispersion and the three-stage sanding dispersion22) 700g/L of slurry, the pH value of the slurry is controlled to be 9.0, and TiO is added2The particle diameter D50 was 0.2 μm, the particle size distribution coefficient PSD was controlled at 0.7, and the rutile conversion R was 98.5%.
b. And (3) drying: adding a polyacrylamide flocculant solution into the TiO2 slurry obtained in the step a under the condition of stirring, wherein the adding amount is TiO20.01 percent of the mass of the flocculant, and 0.1 percent of polyacrylamide is prepared into a flocculant solution with the mass fraction of 0.1 percent. Pumping the flocculated slurry into a filter press for filtering, washing, and drying a filter cake in a flash evaporator to obtain TiO2And (3) powder.
c. Crushing: subjecting the TiO obtained in step b to2Mixing the powder and silane coupling agent in a high-speed mixer, and pulverizing the powder in a steam pulverizer to obtain the final product, wherein the silane coupling agent is TiO20.7% of the mass.
Example 2
a. Preparation of TiO2Slurry preparation: calcining TiO in a rotary kiln2The crude product is dispersed by Raymond mill dry method and three-stage sand mill to prepare the concentration (by TiO)2Calculated) 720g/L of slurry, the pH value of the slurry is controlled to be 9.0, and TiO is added2The particle diameter D50 was 0.21 μm, the particle size distribution coefficient PSD was controlled at 0.8, and the rutile conversion R was 98.5%.
b. And (3) drying: subjecting the TiO obtained in step a to2Directly pumping the slurry into a centrifugal spray dryer for drying to obtain TiO2And (3) powder.
c. Crushing: subjecting the TiO obtained in step b to2Mixing the powder and polydimethylsiloxane uniformly in a high-speed mixer, then feeding the powder into a steam powder machine for crushing to obtain a final product, wherein the addition amount of the polydimethylsiloxane is TiO20.3% of the mass.
Example 3
a. Preparation of TiO2Slurry preparation: calcining TiO in a rotary kiln2The crude product is dispersed by Raymond mill dry method and three-stage sand mill to prepare the concentration (by TiO)2Calculated) 800g/L of slurry, the pH value of the slurry is controlled to be 9.0, and TiO is added2Particle diameter D50 of 0.22 μm, particle size distributionThe coefficient PSD is controlled at 0.9, and the rutile conversion R is 98.5%.
b. And (3) drying: adding the TiO obtained in the step a under the stirring condition2Adding a polyacrylamide flocculant solution into the slurry, wherein the addition amount of the flocculant solution is TiO20.1% of the mass of the flocculant, and 0.1% of polyacrylamide by mass. Pumping the flocculated slurry into a filter press for filtering, washing, and drying a filter cake in a flash evaporator to obtain TiO2And (3) powder.
c. Crushing: subjecting the TiO obtained in step b to2Mixing the powder and organic phosphoric acid in a high-speed mixer, and pulverizing the powder in a steam pulverizer to obtain the final product, wherein the addition amount of the organic phosphoric acid is TiO20.8% of the mass.
Comparative example 1
Comparative example 1 is titanium dioxide powder produced by a certain titanium dioxide powder factory in China, and the process flow is as follows:
a. preparation of TiO2Slurry preparation: adding TiO into the mixture2The crude product is subjected to Raymond mill and sand mill to prepare the concentration (by TiO)2Calculated) 600g/L to 700g/L of slurry, the pH value of the slurry is controlled to be 9 to 10, and TiO2The grain diameter D50 is 0.2-0.22 μm, and the rutile conversion rate R is more than or equal to 98%.
b. Coating with aluminum: subjecting the TiO obtained in step a to2Diluting the slurry to 300-400 g/L (with TiO) with desalted water2Metering), heating the slurry to 50 ℃ by using steam, using sodium hexametaphosphate as a dispersing agent, preparing the sodium hexametaphosphate into a solution with the concentration of 40g/L, and adding the solution in an amount of P2O5Calculated as TiO20.2% of the mass. Adjusting the pH value of the slurry to 9-10, and adding TiO in a parallel flow mode of sodium metaaluminate and dilute sulfuric acid under the stirring condition2Slurry, keeping the pH value of the slurry constant, and adding for 1 hour. Sodium metaaluminate solution concentration is Al2O3Calculated as 100g/L, the addition amount is Al2O3Calculated as TiO21% of the mass, then aging for 1 hour, and adjusting the pH value of the slurry to 7.0.
c. And (3) drying: subjecting the TiO obtained in step b to2Filtering the slurry, washing the filter cake with desalted water to remove soluble salts, making the resistivity of the filter cake be greater than or equal to 150 omega.m, drying the filter cake by using flash evaporator to obtain the invented productAnd (3) powder.
d. Crushing: subjecting the TiO obtained in the step c2Pulverizing the powder with air flow, adding polydimethylsiloxane as organic surface treating agent in TiO amount20.4% of the mass.
Comparative example 2
Titanium dioxide special for certain color master batch in China.
Comparative example 3
Titanium dioxide special for a certain color master batch abroad (Venator product TR-28).
The invention replaces the inorganic aluminum coating process by the process improvement, greatly simplifies the production flow, saves the production cost and has excellent application performance. The examples and comparative examples were subjected to dispersibility, hiding power test and moisture content test, and the results are shown in the following table,
from the data of dispersibility (FPV bar/kg), the dispersibility of the sample in the embodiment is better than that of the domestic masterbatch titanium dioxide, and is close to that of foreign products (the smaller the test data is, the better the dispersibility is), because the number of coarse particles formed in the inorganic coating process is greatly reduced after the aluminum coating is reduced. From the C.R data, the example improves the TiO content in the titanium dioxide2The content, the hiding power of the sample of the example is higher than that of the domestic product, and is equivalent to that of the excellent foreign product. From the ignition loss data at 300 ℃, the amount of crystal water brought by the inorganic aluminum is reduced, and the ignition loss of the samples in the examples is lower than that of the products at home and abroad.
Claims (8)
1. The special titanium dioxide for the color master batch comprises titanium dioxide particles and is characterized in that: the titanium dioxide particles are rutile titanium dioxide particles; the surface of the rutile type titanium dioxide particles is coated with an organic coating, and is not coated with an aluminum coating.
2. The special titanium dioxide for color master batches of claim 1, characterized in that: the organic coating is one or a mixture of silane coupling agent, organic siloxane, silicone oil and organic phosphoric acid.
3. The preparation method of the special titanium dioxide for color master batches as claimed in claim 1, characterized by comprising the following steps:
(1) dry grinding the sulfuric acid process rutile type titanium dioxide crude product to ensure that the particle size of 95 percent of titanium dioxide particles is less than 10 microns;
(2) pulping the titanium dioxide ground by the dry method to obtain TiO2Adding sodium polycarboxylate serving as a dispersing agent into slurry with the concentration of 700 g/L-800 g/L, depolymerizing titanium dioxide coarse particles in the slurry through three-stage sanding, and further removing the large particles from the sanded slurry through a cyclone to obtain sanded slurry;
(3) adding a flocculating agent into the sand grinding slurry obtained in the step (2) to flocculate titanium dioxide particles in the slurry, filtering and washing the flocculated slurry, and drying the slurry by using a flash evaporator to obtain a titanium dioxide intermediate product;
(4) performing steam flow crushing on the titanium dioxide intermediate product obtained in the step (3), and adding an organic coating agent to obtain titanium dioxide special for color master batches; wherein the addition amount of the organic coating agent is TiO20.3-0.8% of the mass.
4. The preparation method of the special titanium dioxide for color master batches as claimed in claim 1, characterized by comprising the following steps:
(1) dry grinding the sulfuric acid process rutile type titanium dioxide crude product to ensure that the particle size of 95 percent of titanium dioxide particles is less than 10 microns;
(2) pulping the titanium dioxide ground by the dry method to obtain TiO2Adding sodium polycarboxylate serving as a dispersing agent into slurry with the concentration of 700 g/L-800 g/L, depolymerizing titanium dioxide coarse particles in the slurry through three-stage sanding, and further removing the large particles from the sanded slurry through a cyclone to obtain sanded slurry;
(3) directly feeding the sand grinding slurry obtained in the step (2) into a centrifugal spray dryer for drying to obtain a titanium dioxide intermediate product;
(4) performing steam flow crushing on the titanium dioxide intermediate product obtained in the step (3), and adding an organic coating agent to obtain titanium dioxide special for color master batches; wherein the addition amount of the organic coating agent is TiO20.3-0.8% of the mass.
5. The preparation method of the special titanium dioxide powder for color master batches according to claim 3 or 4, characterized by comprising the following steps: in step (2), TiO2After sanding, the particle size D50 of the crude product is controlled to be 0.2-0.22 μm, and the particle size distribution coefficient PSD is controlled to be 0.7-0.9.
6. The preparation method of the titanium dioxide special for color master batches as claimed in claim 3, characterized in that: in the step (3), the added flocculating agent is an organic flocculating agent, and the adding amount of the flocculating agent is TiO20.01 to 0.1% by mass.
7. The preparation method of the titanium dioxide special for color master batches as claimed in claim 6, characterized in that: the organic flocculant is a polyacrylamide flocculant.
8. The preparation method of the special titanium dioxide for color master batches according to claim 3 or 4, characterized by comprising the following steps: in the step (4), the organic coating agent is one or a mixture of more of a silane coupling agent, organosiloxane, silicone oil and organic phosphoric acid.
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