CN111073351A - Preparation method of high-weather-resistance and high-dispersion plastic color master batch titanium dioxide pigment - Google Patents
Preparation method of high-weather-resistance and high-dispersion plastic color master batch titanium dioxide pigment Download PDFInfo
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Abstract
A preparation method of a high weather-resistant and high-dispersion plastic color master batch titanium dioxide pigment comprises the steps of producing a titanium dioxide primary product by adopting a chlorination process, pulping in desalted water to prepare a slurry, adjusting the pH value by adopting inorganic acid or alkali, and carrying out dispersion and grinding treatment; heating the slurry, adding an alkaline aluminate compound, maintaining the pH value constant by using inorganic acid or an acidic aluminum compound, and forming an inorganic aluminum film coating layer on the surface of the titanium dioxide particles; adjusting the pH value by adopting an inorganic alkali solution, and adding a polysiloxane liquid containing an active group to form an organic silicon film coating layer; filtering with deionized water, washing, and drying; adding a citrate organic treating agent in the steam-powder process, and obtaining a titanium dioxide finished product after steam-powder treatment. The advantages are that: the titanium dioxide pigment prepared by the method has high weather resistance, high whiteness, high covering power and excellent dispersion processability, is low in dust flying in the production and use processes, is environment-friendly, and is suitable for the high-end color master application fields of polyolefin, engineering plastics and the like.
Description
Technical Field
The invention relates to a preparation method of a high-weather-resistance and high-dispersion plastic color master batch titanium dioxide pigment in the field of chemical industry.
Background
The color master batch is called color master batch, is a special colorant for novel high polymer materials, and is also called a pigment preparation. The color master is mainly used for plastics. The color concentrate is mainly composed of three basic elements of pigment, carrier and additive, and is an aggregate prepared by uniformly loading an excessive amount of pigment into a resin, and can be called pigment concentrate, its tinting strength is higher than that of the pigment itself, and when it is processed, a small amount of color concentrate and uncolored resin are mixed, so that the colored resin or product with designed pigment concentration can be obtained. Has the characteristics of convenient processing, uniform products, easy color matching and the like. The color master batches are classified into color master batches for fibers, color master batches for films, color master batches for wires and cables, polyolefin color master batches, PVC color master batches, color master batches for injection molding products and the like. In recent years, color masterbatch is developing towards multifunction, high pigment content and high technical content, which puts an urgent demand on the improvement of the performance of titanium pigment. Therefore, the surface modification treatment of the plastic color master batch titanium dioxide pigment can improve the dispersion property, the compatibility and the processing property of the titanium dioxide in an application system, thereby becoming a wide technology.
CN 10619716A discloses 'a special titanium dioxide pigment for superfine rutile type color master and a preparation method thereof', the titanium dioxide pigment is produced by adopting a sulfuric acid process, the performance of titanium dioxide is modified by inorganic liquid phase coating and organic silicon film gas-phase coating (vapor powder treatment), the titanium dioxide dispersion problem is mainly solved by organic silicon gas-phase coating, although the dispersion performance of the titanium dioxide in color master application is improved, due to the reasons of small specific gravity of organic silicon substances and the like, dust is generated and flies when an organic silicon treating agent is used in a vapor powder process, and adverse effects are generated on personnel safety and environmental safety; in addition, the organic silicon film vapor-phase coated titanium dioxide pigment has certain influence on yellowing resistance and degradation resistance in the high-temperature processing process of the plastic color master batch.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-weather-resistance and high-dispersity plastic color master batch titanium dioxide pigment, which can keep good yellowing resistance and degradation resistance in the high-temperature plastic processing process of the color master batch under the premise of ensuring the compatibility and the dispersity of a high-plastic system of the titanium dioxide pigment, and the titanium dioxide pigment has the characteristics of high weather resistance, good whiteness and blue bottom phase, and the titanium dioxide pigment prepared by the method effectively solves the dust flying characteristic and has important effects on personnel safety and environmental safety in the production, transportation and application processes.
The technical solution of the invention is as follows:
a preparation method of a high weather resistance and high dispersion plastic color master batch titanium dioxide pigment comprises the following specific steps:
1.1, adding a certain amount of deionized water into a chloride rutile type titanium dioxide primary product to prepare titanium dioxide slurry with the concentration of 300 g/L-500 g/L, adjusting the pH value of the titanium dioxide slurry to 4.5-5.5 by using an inorganic alkali solution, adding a dispersing agent, wherein the adding amount of the dispersing agent is 0.1-0.5 percent of the weight of the titanium dioxide in terms of the effective components of the dispersing agent, and curing for 10-30 min;
1.2, grinding the dispersed titanium dioxide slurry, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40-80 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 to 3.0 percent of alkaline aluminate solution within 30 to 120min, wherein the addition amount of the alkaline aluminate solution is that the alumina accounts for the weight of the titanium dioxide; maintaining the pH value of the slurry to be 4.0-6.0 by using inorganic acid or acidic aluminum salt solution, and curing for 30-60 min to form a first compact aluminum film coating layer;
1.5, continuously adding inorganic alkali solution, adjusting the pH value to 6.5-7.5, and curing for 10-30 min;
1.6, adding polysiloxane liquid in 30-120 min, wherein the polysiloxane has hydroxyl active groups or carboxyl active groups, and curing for 30-60 min to form a polymerized silicon film coating layer;
1.7, washing the solution with deionized water at 70-90 ℃ until the electric conductivity of a filter cake is more than 15000 omega cm, and drying;
1.8, adding a citrate organic treating agent in the steam powder process to prepare the titanium dioxide pigment for the plastic color master batch.
Further, the dispersant in 1.1 is a silicate dispersant or a phosphate dispersant.
Further, the alkaline aluminum salt solution in 1.4 is a sodium metaaluminate solution or a potassium metaaluminate solution; the concentration of the alkaline aluminum salt solution is Al2O3The weight is 100 g/L-200 g/L.
Further, the acidic aluminum salt solution in 1.4 is one of an aluminum sulfate solution, an aluminum trichloride solution and an aluminum nitrate solution; concentration of acidic aluminum salt solution is as Al2O3The weight is 60g/L to 120 g/L.
Further, the inorganic acid in 1.4 is one of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid; the mass concentration of the inorganic acid is 10-30%.
Further, the inorganic alkali solution in 1.1 and 1.5 is sodium hydroxide solution or potassium hydroxide solution, and the mass concentration of the inorganic alkali solution is 10-30%.
Furthermore, the polysiloxane liquid is added in an amount of 0.5 to 1.5 percent of the weight of the titanium dioxide based on the solid content of the polysiloxane.
Further, 1.8 of the citric acid ester organic treating agent is tributyl citrate or acetyl tributyl citrate, and the addition amount of the citric acid ester organic treating agent is that the carbon content accounts for 0.1-1.0% of the weight of the titanium dioxide.
Furthermore, the content of rutile in the titanium dioxide primary product is more than 99.5%, and the particle size of D50 is 0.20-0.28 μm.
Furthermore, after the grinding treatment in the step 1.2, the particle size of the titanium dioxide D50 is 280-287 nm, and the particle size of the titanium dioxide D50 with the particle size of more than 500nm is less than 5.5%.
Compared with the prior art, the invention has the beneficial effects that:
(1) the chloride process rutile type titanium dioxide oxidation primary product is used as a raw material for preparing a target product, and has the characteristics of high approximately spherical proportion of particles, small particle size and narrow particle size distribution.
(2) Proper cladding layer combination is adopted, wherein a first dense aluminum film layer is formed by adopting a basic aluminum salt solution and an inorganic acid or acidic aluminum salt solution and controlling and adjusting the pH value, so that the photochemical active points of titanium dioxide are effectively compensated, and the anti-discoloration performance is improved; and adding polysiloxane pure liquid or emulsion into the titanium dioxide slurry, and forming a second coating layer of the polymerized silicon film through hydroxyl or carboxyl groups and hydroxyl groups on the surface of the first coating layer. Compared with a vapor-phase coating film, the liquid-phase coating of the organic silicon film is more uniform and complete, and is chemically bonded on the surface of the titanium dioxide, so that the formed coating layer is firm, and the characteristic of high content of crystal water in the liquid-phase coating of the inorganic silicon oxide film is reduced on the premise of improving the weather resistance of the product.
(3) The high-temperature-resistant citrate organic agent is introduced in the steam-powder process, so that the grinding aid is played, and the key point is that the lipid dispersing agent is introduced along with steam and is coated on the surfaces of titanium dioxide particles, so that the compatibility of titanium dioxide and plastic resin is effectively improved.
(4) According to the method, on the basis of the traditional aluminum oxide coating, the active group is chemically bonded and coated on the compact organic silicon film, so that the content of hydroxyl-bound water can be reduced to the maximum extent, the hydrophilic surface of titanium dioxide is converted into a hydrophobic surface, the content of adsorbed water is reduced, and the influence of yellowing resistance and degradation resistance of bound water in the high-temperature plastic processing process is fundamentally solved; the ester treating agent is used as the outer organic coating layer, so that the problem of flying titanium dioxide dust is solved, the compatibility of the titanium dioxide and resin is further enhanced, and the system dispersibility and the processability of the titanium dioxide are improved. The unqualified phenomena of white spots, plaques and other products caused by system incompatibility and poor dispersion are effectively avoided. The obtained product has high weather resistance, high whiteness, high compatibility and dispersibility of a plastic system, and ensures excellent processing performance and mechanical property of the plastic product.
Detailed Description
The present invention will be further described with reference to the following embodiments, but the application scope of the present invention is not limited to the embodiments, and various substitutions and modifications can be made without departing from the technical idea of the present invention.
Example 1
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 300g/L, wherein the content of rutile in the titanium dioxide primary product is 99.5%, and the particle size of D50 is 0.20 mu m; adjusting the pH value of the titanium dioxide slurry to 4.5 by using a sodium hydroxide solution with the mass concentration of 30 percent, and adding a 0.1 percent sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 10min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 280nm, the particle size of particles with the particle size of more than 500nm is less than 5.0 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 percent NaAlO within 30min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 200 g/L; with combined use of Al2(SO4)3Solution maintenance of slurry pH4.0 concentration of acidic aluminum salt solution as Al2O3The mixture is aged for 30min at the concentration of 100g/L to form a first compact aluminum film coating layer;
1.5, adding NaOH solution with the mass concentration of 30%, adjusting the pH value to 6.5, and curing for 10 min;
1.6, adding 0.5 percent of hydroxyl polysiloxane liquid (the adding amount of the hydroxyl polysiloxane liquid is that the solid content of the hydroxyl polysiloxane accounts for the weight of the titanium dioxide) in 30min, and curing for 30 min;
1.7, washing the solution with deionized water at 70 ℃ until the electric conductivity of a filter cake is 16000 omega-cm, and drying;
1.8, adding a tributyl citrate organic treating agent (the addition of the tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide) in the steam powder process to prepare the titanium dioxide pigment for the plastic color master batch.
Example 2
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 500g/L, wherein the content of rutile in the titanium dioxide primary product is 99.7%, and the particle size of D50 is 0.28 mu m; adjusting the pH value of the titanium dioxide slurry to 5.5 by using a sodium hydroxide solution with the mass concentration of 10 percent, and adding a 0.5 percent sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 30min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the particle size of D50 is 287nm, and the particle size of particles with the particle size of more than 500nm is less than 5.3 percent, and removing a grinding medium from the water slurry;
1.3, heating the ground slurry to 80 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 3.0 percent NaAlO within 30min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 100 g/L; maintaining the pH value of the slurry to be 6.0 by using HCI solution with the mass concentration of 15%, and curing for 60min to form a first compact aluminum film coating layer;
1.5, adding KOH solution with the mass concentration of 10%, adjusting the pH value to 7.5, and curing for 30 min;
1.6, adding 1.5 percent of carboxyl polysiloxane liquid (the adding amount of the carboxyl polysiloxane liquid is that the solid content of the carboxyl polysiloxane accounts for the weight of the titanium dioxide) in 120min, and curing for 60 min;
1.7, washing the solution with deionized water at 90 ℃ until the conductivity of a filter cake is 17000 omega cm, and drying;
1.8, adding an acetyl tributyl citrate organic treating agent in the steam powder process (the addition of the acetyl tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide), and preparing the titanium dioxide pigment for the plastic color master batch.
Example 3
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 400g/L, wherein the content of rutile in the titanium dioxide primary product is 99.9 percent, and the particle size of D50 is 0.25 mu m; adjusting the pH value of the titanium dioxide slurry to 5.0 by using a sodium hydroxide solution with the mass concentration of 20%, and adding a 0.3% sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 20min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 285nm, the particle size of particles with the particle size of more than 500nm is less than 5.5 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 60 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 2.0 percent NaAlO within 120min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 150 g/L; using 30% H by mass2SO4Maintaining the pH value of the slurry to be 5.0, and curing for 40min to form a first compact aluminum film coating layer;
1.5, adding NaOH solution with the mass concentration of 20%, adjusting the pH value to 7.0, and curing for 20 min;
1.6, adding 1.0 percent of hydroxyl-terminated polysiloxane liquid (the adding amount is that the solid content of the hydroxyl-terminated polysiloxane accounts for the weight of the titanium dioxide) in 30min, and curing for 40 min;
1.7, washing the solution with deionized water at the temperature of 80 ℃ until the conductivity of a filter cake is 15600 omega cm, and drying;
1.8, adding a tributyl citrate organic treating agent (the addition of the tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide) in the steam powder process to prepare the titanium dioxide pigment for the plastic color master batch.
Comparative example 1 the inorganic treatment procedure of example 1 was repeated, eliminating the first inorganic alumina coating procedure.
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 300g/L, wherein the content of rutile in the titanium dioxide primary product is 99.5%, and the particle size of D50 is 0.20 mu m; adjusting the pH value of the titanium dioxide slurry to 4.5 by using a sodium hydroxide solution with the mass concentration of 30 percent, and adding a 0.1 percent sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 10min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 280nm, the particle size of particles with the particle size of more than 500nm is less than 5.0 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40 ℃, and maintaining the temperature in the whole coating process;
1.4, adding NaOH solution with the mass concentration of 30%, adjusting the pH value to 6.5, and curing for 10 min;
1.5, adding 0.5 percent of hydroxyl polysiloxane liquid (the adding amount of the hydroxyl polysiloxane liquid is that the solid content of the hydroxyl polysiloxane accounts for the weight of the titanium dioxide) in 30min, and curing for 30 min;
1.6, washing the solution with deionized water at 70 ℃ until the electric conductivity of a filter cake is 16000 omega-cm, and drying;
1.7, adding a tributyl citrate organic treating agent in the steam-powder process (the addition of the tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide) to prepare the titanium dioxide pigment.
Comparative example 2 the inorganic treatment procedure of example 1 was repeated, eliminating the 1.6 step second silicone film coating procedure.
1.1 rutile-type dioxygen produced by ChlorinationDissolving a titanium primary product, and adding a certain amount of deionized water to prepare titanium dioxide slurry with the concentration of 300g/L, wherein the content of rutile in the titanium dioxide primary product is 99.5%, and the particle size of D50 is 0.20 mu m; adjusting the pH value of the titanium dioxide slurry to 4.5 by using a sodium hydroxide solution with the mass concentration of 30 percent, and adding a 0.1 percent sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 10min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 280nm, the particle size of particles with the particle size of more than 500nm is less than 5.0 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 percent NaAlO within 30min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 200 g/L; with combined use of Al2(SO4)3The pH value of the slurry is maintained to be 4.0, and the concentration of the acidic aluminum salt solution is Al2O3The mixture is aged for 30min at the concentration of 100g/L to form a first compact aluminum film coating layer;
1.5, washing the solution with deionized water at 70 ℃ until the electric conductivity of a filter cake is 16000 omega-cm, and drying;
1.6, adding a tributyl citrate organic treating agent (the addition of the tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide) in the steam-powder process to prepare the titanium dioxide pigment for the plastic color master batch.
Comparative example 3 the inorganic treatment procedure of example 1 was repeated to change the hydroxy polysiloxane liquid of step 1.6 to a sodium silicate solution in an amount of SiO2Is TiO 221.0% by weight, concentration in SiO2The weight is 150 g/L.
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 300g/L, wherein the content of rutile in the titanium dioxide primary product is 99.5%, and the particle size of D50 is 0.20 mu m; adjusting the pH value of the titanium dioxide slurry to 4.5 by using 30 mass percent sodium hydroxide solution, and adding 0.1 mass percent sodium silicate solutionLiquid (sodium silicate solution added in SiO2Is TiO 22By weight), sodium silicate solution in SiO2Aging for 10min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 280nm, the particle size of particles with the particle size of more than 500nm is less than 5.0 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 percent NaAlO within 30min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 200 g/L; with combined use of Al2(SO4)3The pH value of the slurry is maintained to be 4.0, and the concentration of the acidic aluminum salt solution is Al2O3The mixture is aged for 30min at the concentration of 100g/L to form a first compact aluminum film coating layer;
1.5, adding NaOH solution with the mass concentration of 30%, adjusting the pH value to 6.5, and curing for 10 min;
1.6, adding 0.5 percent of hydroxyl polysiloxane liquid (the adding amount of the hydroxyl polysiloxane liquid is that the solid content of the hydroxyl polysiloxane accounts for the weight of the titanium dioxide) in 30min, and curing for 30 min;
1.7, washing the solution with deionized water at 70 ℃ until the electric conductivity of a filter cake is 16000 omega-cm, and drying;
1.8, adding a tributyl citrate organic treating agent (the addition of the tributyl citrate is that the carbon content accounts for 1.0 percent of the weight of the titanium dioxide) in the steam powder process to prepare the titanium dioxide pigment for the plastic color master batch.
Comparative example 4 the inorganic treatment procedure of example 1 was repeated, eliminating the 1.8 step outer organic coating procedure.
1.1, adding a certain amount of deionized water into a rutile type titanium dioxide primary product by adopting a chlorination method to prepare titanium dioxide slurry with the concentration of 300g/L, wherein the content of rutile in the titanium dioxide primary product is 99.5%, and the particle size of D50 is 0.20 mu m; adjusting the pH value of the titanium dioxide slurry to 4.5 by using a sodium hydroxide solution with the mass concentration of 30 percent, and adding a 0.1 percent sodium silicate solution (the adding amount of the sodium silicate solution is SiO2Is TiO 22By weight), silicic acidSodium solution with SiO2Aging for 10min, wherein the amount is 150 g/L;
1.2, grinding the dispersed titanium dioxide slurry, wherein the D50 particle size is 280nm, the particle size of particles with the particle size of more than 500nm is less than 5.0 percent, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 percent NaAlO within 30min2Solution (the addition amount is calculated by the weight of alumina in titanium dioxide), and the concentration of sodium metaaluminate solution is calculated by Al2O3The weight is 200 g/L; with combined use of Al2(SO4)3The pH value of the slurry is maintained to be 4.0, and the concentration of the acidic aluminum salt solution is Al2O3The mixture is aged for 30min at the concentration of 100g/L to form a first compact aluminum film coating layer;
1.5, adding NaOH solution with the mass concentration of 30%, adjusting the pH value to 6.5, and curing for 10 min;
1.6, adding 0.5 percent of hydroxyl polysiloxane liquid (the adding amount of the hydroxyl polysiloxane liquid is that the solid content of the hydroxyl polysiloxane accounts for the weight of the titanium dioxide) in 30min, and curing for 30 min;
1.7, washing the solution with deionized water at 70 ℃ until the electric conductivity of a filter cake is 16000 omega-cm, drying, and carrying out vapor-powder treatment to obtain the titanium dioxide pigment for the plastic color master batch.
The polysiloxane used in the embodiment of the present invention has a carboxyl-reactive group or a hydroxyl-reactive group, and forms a coating film by the carboxyl/hydroxyl-reactive group and a hydroxyl group on the surface of the first coating layer.
The titanium dioxide pigments prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to a plastic system application property test, and the test results are shown in table 1.
The method is characterized in that weather resistance delta E detection is a result of irradiation of a prepared standard plastic plate for 240 hours under a xenon lamp aging box (UVA) lamp, a yellowing index 240h (△ E) is a result of irradiation of the prepared standard plastic plate for 240 hours under the UVA lamp, tensile strength and impact strength are 60% of test values of the ABS master batch prepared plastic plate, dust flying conditions occur, and the method is used for judging the dust flying conditions by personnel working in production lines for a long time.
As can be seen from table 1: the dispersibility, weather resistance, discoloration resistance and material mechanical properties of the products prepared in the embodiments 1 to 3 are obviously improved, and all index properties are excellent. Comparative example 1 no alumina coating was performed and the yellowing resistance of the product was poor; comparative example 2 is not coated with the organic silicon film, the product has poor filter pressure value dispersibility and weather resistance, and the product has poor material performance due to insufficient dispersion; comparative example 3 adopts inorganic silicon to replace organic silicon for coating, and various indexes are not ideal due to the existence of multiple binding water and adsorption water; comparative example 4, no outer organic coating was performed, titanium dioxide dust was flying seriously, and the environment was not friendly. And the dispersion and mechanical properties of the material are reduced due to insufficient compatibility with the applied resin.
In conclusion, the titanium dioxide pigment produced according to the invention has high dispersibility, high weather resistance, excellent discoloration resistance, excellent material processability and excellent mechanical properties, and is suitable for the high-end color master batch application fields of polyolefin, engineering plastics and the like.
The above description is only an example of the present invention and is not intended to limit the present invention, and it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a high weather resistance and high dispersion plastic color master batch titanium dioxide pigment is characterized by comprising the following steps:
1.1, adding a certain amount of deionized water into a chloride rutile type titanium dioxide primary product to prepare titanium dioxide slurry with the concentration of 300 g/L-500 g/L, adjusting the pH value of the titanium dioxide slurry to 4.5-5.5 by using an inorganic alkali solution, adding a dispersing agent, wherein the adding amount of the dispersing agent is 0.1-0.5 percent of the weight of the titanium dioxide in terms of the effective components of the dispersing agent, and curing for 10-30 min;
1.2, grinding the dispersed titanium dioxide slurry, and removing grinding media from the water slurry;
1.3, heating the ground slurry to 40-80 ℃, and maintaining the temperature in the whole coating process;
1.4, adding 0.5 to 3.0 percent of alkaline aluminate solution within 30 to 120min, wherein the addition amount of the alkaline aluminate solution is that the alumina accounts for the weight of the titanium dioxide; maintaining the pH value of the slurry to be 4.0-6.0 by using inorganic acid or acidic aluminum salt solution, and curing for 30-60 min to form a first compact aluminum film coating layer;
1.5, continuously adding inorganic alkali solution, adjusting the pH value to 6.5-7.5, and curing for 10-30 min;
1.6, adding polysiloxane liquid in 30-120 min, wherein the polysiloxane has hydroxyl active groups or carboxyl active groups, and curing for 30-60 min to form a polymerized silicon film coating layer;
1.7, washing the solution with deionized water at 70-90 ℃ until the electric conductivity of a filter cake is more than 15000 omega cm, and drying;
1.8, adding a citrate organic treating agent in the steam powder process to prepare the titanium dioxide pigment for the plastic color master batch.
2. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: 1.1 the dispersant is a silicate dispersant or a phosphate dispersant.
3. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: 1.4, the alkaline aluminum salt solution is a sodium metaaluminate solution or a potassium metaaluminate solution; the concentration of the alkaline aluminum salt solution is Al2O3The weight is 100 g/L-200 g/L.
4. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: 1.4 the acidic aluminum salt solution is one of aluminum sulfate solution, aluminum trichloride solution and aluminum nitrate solution(ii) a Concentration of acidic aluminum salt solution is as Al2O3The weight is 60g/L to 120 g/L.
5. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: 1.4, the inorganic acid is one of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid; the mass concentration of the inorganic acid is 10-30%.
6. The method for preparing the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: the inorganic alkali solution in 1.1 and 1.5 is sodium hydroxide solution or potassium hydroxide solution, and the mass concentration of the inorganic alkali solution is 10-30%.
7. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: the addition amount of the polysiloxane liquid is 0.5-1.5% of the weight of titanium dioxide based on the solid content of polysiloxane.
8. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: 1.8 the citrate organic treating agent is tributyl citrate or acetyl tributyl citrate, and the addition amount of the citrate organic treating agent is that the carbon content accounts for 0.1-1.0 percent of the weight of the titanium dioxide.
9. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: the content of rutile in the titanium dioxide primary product is more than 99.5%, and the particle size of D50 is 0.20-0.28 μm.
10. The preparation method of the high weather resistance and high dispersion plastic color master batch titanium dioxide pigment according to claim 1, which is characterized in that: after the grinding treatment in the step 1.2, the particle size of the titanium dioxide D50 is 280-287 nm, and the particle size of the titanium dioxide D50 which exceeds 500nm is less than 5.5%.
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| CN103013184A (en) * | 2012-12-29 | 2013-04-03 | 锦州钛业有限公司 | Preparation method of special type titanium dioxide pigment for plastic color master batch |
| CN110157219A (en) * | 2019-06-26 | 2019-08-23 | 河南佰利联新材料有限公司 | A kind of preparation method of high-performance Masterbatch special titanium pigment |
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| US20090286901A1 (en) * | 2005-04-26 | 2009-11-19 | Cornelis Adrianus Maria Vijverberg | Coated particles and coating compositions comprising coated particles |
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| CN103013184A (en) * | 2012-12-29 | 2013-04-03 | 锦州钛业有限公司 | Preparation method of special type titanium dioxide pigment for plastic color master batch |
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