CN111909545A - Titanium white chloride special for plastic color master batch and preparation method thereof - Google Patents

Titanium white chloride special for plastic color master batch and preparation method thereof Download PDF

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CN111909545A
CN111909545A CN202010871148.8A CN202010871148A CN111909545A CN 111909545 A CN111909545 A CN 111909545A CN 202010871148 A CN202010871148 A CN 202010871148A CN 111909545 A CN111909545 A CN 111909545A
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slurry
plastic color
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titanium white
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肖勇丽
淦文军
赵北东
喻晖
曹磊
柳令
李开娟
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Chongqing Panzhihua Iron And Steel Group Co ltd
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Abstract

The invention belongs to the technical field of preparation of titanium white chloride, and particularly relates to a special titanium white chloride for plastic color masterbatch and a preparation method thereof. Aiming at the problem that the titanium dioxide produced by the existing method can not meet the requirements of plastic color master batch products on safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and other properties, the invention provides a preparation method of special titanium chloride white for plastic color master batch, which comprises the following steps: a. adding water and a dispersant into a pulping tank; b. adding a titanium dioxide primary product, and adjusting the concentration of the slurry to 300-800 g/L; c. grinding, depolymerizing and filtering; d. diluting the slurry to 200-300 g/L, and stirring and dispersing for 50-150 min; e. adding aluminum sulfate for coating; f. filtering, drying, crushing, and adding a phosphonic acid solution in a concurrent flow manner to obtain the titanium white special for the high-end plastic color master batch. The titanium dioxide prepared by the method has good hue and dispersibility, and also has good performances of safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and the like, and can meet the requirements of the high-end plastic color masterbatch field.

Description

Titanium white chloride special for plastic color master batch and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of titanium white chloride, and particularly relates to a special titanium white chloride for plastic color masterbatch and a preparation method thereof.
Background
Titanium dioxide is used as the best white pigment, and the color phase is the key. Compared with sulfuric acid method titanium white, the chlorination method titanium white product has better hue, more uniform particle size and distribution, and can meet the requirements of high-end plastic field on the hue and the dispersity of titanium white. In addition, compared with the production process of titanium white by a sulfuric acid method, the production process of titanium white by a chlorination method has fewer waste byproducts and is more beneficial to environmental protection. At present, the application of plastic color masterbatch products in the fields of household appliances, medicine and health, aerospace and aviation and the like is increased year by year, and the fields not only require hue and dispersity, but also provide higher requirements for safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and the like of the plastic color masterbatch products (the requirements of RoHS instruction, REACH regulation, PAHs polycyclic aromatic hydrocarbon, food grade detection (FDA, LFGB and GB food grade), CQC certification, UL certification and the like are met, the processing temperature is more than or equal to 260 ℃, the oxygen index is more than 30 percent, and delta E before and after ultraviolet aging is less than or equal to 0.8). Titanium dioxide is used as a main raw material of a plastic color master batch product, the quality level of the titanium dioxide plays a decisive role in the performance of the plastic color master batch product, and the common titanium dioxide product cannot meet the special requirements of the high-end plastic color master batch industry.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the titanium dioxide produced by the existing method can not meet the requirements of the plastic color master batch products on safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and other properties.
The technical scheme for solving the technical problems comprises the following steps: provides a preparation method of titanium white chloride special for plastic color master batch. The method comprises the following steps:
a. adding water into a pulping tank, and adding a pulping dispersant under the stirring condition, wherein the addition amount of the pulping dispersant is 0.1-0.5% of the content of titanium dioxide;
b. adding the titanium dioxide primary product by the chlorination process into a pulping tank, adding water until the concentration of the slurry is 300-800 g/L, and stirring and dispersing for 30-60 min;
c. b, transferring the slurry obtained in the step b into a sand mill for grinding and depolymerization, and filtering the depolymerized slurry through a screen with 200-800 meshes to obtain filtered slurry;
d. diluting the filtered slurry obtained in the step c to 200-300 g/L with water, heating and maintaining the system temperature at 50-80 ℃, adding dilute alkali liquor into the slurry at a constant speed within 50-150 min to adjust the pH value of the slurry to 5-7, and stirring and dispersing for 50-150 min;
e. d, adding an aluminum sulfate solution and a dilute alkali liquor into the slurry obtained in the step d at a constant speed in a parallel flow mode within 30-120 min, controlling the pH value of the slurry to be 5-7, stirring and dispersing for 50-150 min, and coating;
f. and e, filtering the slurry obtained in the step e by using a 200-800-mesh screen, washing to obtain a filter cake, drying and crushing the filter cake, and adding a phosphonic acid solution into the filter cake in a concurrent flow manner to obtain the titanium white special for the high-end plastic color master.
In the preparation method of the titanium white chloride special for the plastic color master batch, the pulping dispersant in the step a is modified polycarboxylate.
Wherein, in the preparation method of the titanium dioxide chloride special for the plastic color master batch, TiO in the titanium dioxide primary product by the chlorination process in the step b2The content of (A) is more than or equal to 95 percent.
In the preparation method of the titanium chloride white special for the plastic color master, the slurry obtained in the step c is subjected to grading treatment, the particle size D50 of titanium dioxide particles in the graded slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
Wherein, in the preparation method of the titanium chloride white special for the plastic color master batch, the adding amount of the aluminum sulfate solution in the step d is Al2O3Measured as TiO in the slurry20.5 to 1.5% by mass.
In the preparation method of the titanium chloride white special for the plastic color master batch, the volume concentration of the dilute alkali liquor in the steps c and d is 8-15%.
In the preparation method of the titanium chloride white special for the plastic color master batch, the phosphonic acid content in the phosphonic acid solution in the step f is more than or equal to 70%.
Preferably, in the preparation method of the titanium white chloride special for the plastic color master batch, the phosphonic acid solution in the step f is an octylphosphonic acid solution.
Wherein, in the preparation method of the titanium white chloride special for the plastic color master batch, the adding amount of the phosphonic acid solution in the step f is TiO20.3 to 1.5% by mass.
In the preparation method of the titanium white chloride special for the plastic color master batch, the water is deionized water or distilled water.
The invention also provides the titanium white chloride special for the plastic color master batch prepared by the preparation method.
Wherein, in the titanium chloride white special for the plastic color master batch, the high-temperature volatile matter at 300 ℃ is less than or equal to 0.3 percent, the dispersity in a PP resin system is less than or equal to 0.3bar/g, the L value in the PP resin system is more than or equal to 94.50, the b value is less than or equal to 0.50, and the QUV aging resistant color difference delta E is less than or equal to 0.50.
The invention has the beneficial effects that:
the invention provides a preparation method of titanium white chloride special for plastic color master batch, which combines a plurality of means such as selection of titanium dioxide primary product raw materials, selection of a special dispersing agent, classification treatment, alkali liquor pretreatment, phosphonic acid solution organic treatment and the like, so that the obtained titanium white chloride has good hue and dispersibility, and simultaneously has good performances such as safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and the like, and can meet the requirements of the high-end plastic color master batch field. The invention develops a new titanium white chloride and a preparation method thereof for the field of high-end plastic color master batch, has simple operation, low equipment requirement and obvious economic benefit, and is suitable for popularization and use.
Detailed Description
The invention provides a preparation method of special titanium chloride white for plastic color master batch, which comprises the following steps:
a. adding water into a pulping tank, and adding a pulping dispersant under the stirring condition, wherein the addition amount of the pulping dispersant is 0.1-0.5% of the content of titanium dioxide;
b. adding the titanium dioxide primary product by the chlorination process into a pulping tank, adding water until the concentration of the slurry is 300-800 g/L, and stirring and dispersing for 30-60 min;
c. b, transferring the slurry obtained in the step b into a sand mill for grinding and depolymerization, and filtering the depolymerized slurry through a screen with 200-800 meshes to obtain filtered slurry;
d. diluting the filtered slurry obtained in the step c to 200-300 g/L with water, heating and maintaining the system temperature at 50-80 ℃, adding dilute alkali liquor into the slurry at a constant speed within 50-150 min to adjust the pH value of the slurry to 5-7, and stirring and dispersing for 50-150 min;
e. d, adding an aluminum sulfate solution and a dilute alkali liquor into the slurry obtained in the step d at a constant speed in a parallel flow mode within 30-120 min, controlling the pH value of the slurry to be 5-7, stirring and dispersing for 50-150 min, and coating;
f. and e, filtering the slurry obtained in the step e by using a 200-800-mesh screen, washing to obtain a filter cake, drying and crushing the filter cake, and adding a phosphonic acid solution into the filter cake in a concurrent flow manner to obtain the titanium white special for the high-end plastic color master.
In the preparation method of the titanium white chloride special for the plastic color master batch, the pulping dispersant in the step a is modified polycarboxylate. The modified polycarboxylate is used as the pulping dispersant for the first time, compared with the existing dispersant, the modified polycarboxylate does not contain nitrogen and phosphorus, is beneficial to environmental protection, does not need to add acid or alkali to adjust the pH value of the pulp, simplifies the pulping process and reduces the cost.
Wherein, in the preparation method of the titanium white chloride special for the plastic color master batch, the chlorination process is adopted for oxidationTiO in titanium primary products2The content of (A) is more than or equal to 95 percent.
In the preparation method of the titanium chloride white special for the plastic color master, the slurry obtained in the step c is subjected to grading treatment, the particle size D50 of titanium dioxide particles in the graded slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
According to the invention, the sizing agent is graded, and the particle size D50 of titanium dioxide particles in the graded sizing agent is finally determined to be 0.25-0.45 mu m and D90 is less than or equal to 0.8 mu m through a large number of screening tests.
In addition, the invention also adopts alkali liquor to carry out pretreatment on the depolymerized titanium dioxide slurry, ensures that all aluminum is uniformly and compactly coated on the surface of titanium dioxide particles in the form of an amorphous alumina film, reduces the high-temperature volatile matter of titanium white, and improves the ultraviolet aging resistance of the titanium white.
Wherein, in the preparation method of the titanium chloride white special for the plastic color master batch, the adding amount of the aluminum sulfate solution in the step d is Al2O3Measured as TiO in the slurry20.5 to 1.5% by mass.
In the preparation method of the titanium chloride white special for the plastic color master batch, the volume concentration of the dilute alkali liquor in the steps c and d is 8-15%.
Furthermore, the invention also adopts phosphonic acid solution to carry out organic treatment on the titanium dioxide particles, thereby reducing the high-temperature volatile matter of the titanium white and reducing the burning explosion performance of the plastic color master batch product. In the preparation method of the titanium chloride white special for the plastic color master batch, the phosphonic acid content in the phosphonic acid solution in the step f is more than or equal to 70%.
Preferably, in the preparation method of the titanium white chloride special for the plastic color master batch, the phosphonic acid solution in the step f is an octylphosphonic acid solution.
Wherein, in the preparation method of the titanium white chloride special for the plastic color master batch, the adding amount of the phosphonic acid solution in the step f is TiO20.3 to 1.5% by mass.
The invention also provides the titanium white chloride special for the plastic color master batch prepared by the preparation method.
Wherein, in the titanium chloride white special for the plastic color master batch, the high-temperature volatile matter at 300 ℃ is less than or equal to 0.3 percent, the dispersity in a PP resin system is less than or equal to 0.3bar/g, the L value in the PP resin system is more than or equal to 94.50, the b value is less than or equal to 0.50, and the QUV aging resistant color difference delta E is less than or equal to 0.50.
The invention provides a preparation method of titanium dioxide chloride special for high-end plastic color master batch, and the titanium dioxide prepared by the method has excellent performance in the field of plastic color master batch, can meet the requirements of the high-end plastic color master batch field on the hue and the dispersibility of the titanium dioxide, and can also meet the special requirements of the titanium dioxide on safety, environmental protection, high temperature resistance, flame retardance, ultraviolet aging resistance and the like.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
Example 1
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.25 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 550g/L, and stirring and dispersing for 45 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 500-mesh screen to obtain filtered pulp;
4. and classifying the filtered slurry by using a cyclone classifier, wherein the particle size D50 of titanium dioxide particles in the classified slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
5. Adding the slurry meeting the requirements into coating equipment with a stirring device, starting stirring, diluting the slurry to 250g/L by using deionized water or distilled water, heating and maintaining the system temperature at 65 ℃, adding 12% of dilute alkali liquor into the slurry at a constant speed within 100 minutes to adjust the pH value of the slurry to 6.0, and stirring and dispersing for 100 minutes;
6. in thatAdding aluminum sulfate solution and 12 percent of dilute alkali liquor into the slurry at constant speed and in parallel flow within 80 minutes, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry2The mass is 1.0 percent, the pH value of the slurry is controlled to be 6.0, and the slurry is stirred and dispersed for 100 minutes;
7. filtering the obtained slurry by a 500-mesh screen, washing the slurry by deionized water or distilled water to obtain a filter cake, drying the filter cake, crushing the dried material, and simultaneously adding 75% of octyl phosphonic acid solution in a concurrent flow manner, wherein the addition amount of the octyl phosphonic acid solution is TiO20.8 percent of the mass, and the crushed material is the titanium white chloride 1 special for the plastic color master batch.
Example 2
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.1 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 300g/L, and stirring and dispersing for 30 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 200-mesh screen to obtain filtered pulp;
4. and classifying the filtered slurry by using a cyclone classifier, wherein the particle size D50 of titanium dioxide particles in the classified slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
5. Adding the slurry meeting the requirements into coating equipment with a stirring device, starting stirring, diluting the slurry to 200g/L by using deionized water or distilled water, heating and maintaining the temperature of the system at 50 ℃, adding 8% of dilute alkali liquor into the slurry at a constant speed within 50 minutes to adjust the pH value of the slurry to 5.0, and stirring and dispersing for 50 minutes;
6. adding aluminum sulfate solution and 8% dilute alkali liquor into the slurry at constant speed and in parallel flow within 30min, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry20.5 percent of the mass, and the pH value of the slurry is controlled to be 5.0Stirring and dispersing for 50 minutes;
7. filtering the obtained slurry by a 200-mesh screen, washing the slurry by deionized water or distilled water to obtain a filter cake, drying the filter cake, crushing the dried material, and simultaneously adding 70% of octyl phosphonic acid solution in a concurrent flow manner, wherein the addition amount of the octyl phosphonic acid solution is TiO20.3 percent of the mass, and the crushed material is the titanium white chloride 2 special for the plastic color master batch.
Example 3
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.5 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 800g/L, and stirring and dispersing for 60 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 800-mesh screen to obtain filtered pulp;
4. and classifying the filtered slurry by using a cyclone classifier, wherein the particle size D50 of titanium dioxide particles in the classified slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
5. Adding the slurry meeting the requirements into coating equipment with a stirring device, starting stirring, diluting the slurry to 300g/L by using deionized water or distilled water, heating and maintaining the system temperature at 80 ℃, adding 15% of dilute alkali liquor into the slurry at a constant speed within 150 minutes to adjust the pH value of the slurry to 7.0, and stirring and dispersing for 150 minutes;
6. adding aluminum sulfate solution and 15% dilute alkali liquor into the slurry at constant speed in a concurrent flow manner within 120 minutes, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry2The mass is 1.5 percent, the pH value of the slurry is controlled to be 7.0, and the slurry is stirred and dispersed for 150 minutes;
7. filtering the obtained slurry with 800 mesh screen, washing with deionized water or distilled water to obtain filter cake, drying the filter cake, and pulverizingSimultaneously adding 80 percent of octyl phosphonic acid solution in a concurrent flow manner, wherein the adding amount of the octyl phosphonic acid solution is TiO calculated by phosphonic acid21.5 percent of the mass, and the crushed material is the titanium white chloride special for the plastic color master batch 3.
Comparative example 1
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.25 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 550g/L, and stirring and dispersing for 45 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 500-mesh screen to obtain filtered pulp;
4. adding the filtered slurry into coating equipment with a stirring device, starting stirring, diluting the slurry to 250g/L by using deionized water or distilled water, heating and maintaining the system temperature at 65 ℃, adding 12% of dilute alkali liquor into the slurry at a constant speed within 100 minutes to adjust the pH value of the slurry to 6.0, and stirring and dispersing for 100 minutes;
6. adding aluminum sulfate solution and 12 percent of dilute alkali liquor into the slurry at constant speed and in parallel flow within 80 minutes, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry2The mass is 1.0 percent, the pH value of the slurry is controlled to be 6.0, and the slurry is stirred and dispersed for 100 minutes;
7. filtering the obtained slurry by a 500-mesh screen, washing the slurry by deionized water or distilled water to obtain a filter cake, drying the filter cake, crushing the dried material, and simultaneously adding 75% of octyl phosphonic acid solution in a concurrent flow manner, wherein the addition amount of the octyl phosphonic acid solution is TiO calculated by phosphonic acid20.8 percent of the mass, and the crushed material is the titanium white chloride 4 special for the plastic color master batch.
Comparative example 2
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.25 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 550g/L, and stirring and dispersing for 45 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 500-mesh screen to obtain filtered pulp;
4. adding the filtered slurry into coating equipment with a stirring device, starting stirring, diluting the slurry to 250g/L by using deionized water or distilled water, heating and maintaining the system temperature at 65 ℃, adding an aluminum sulfate solution and 12% dilute alkali liquor into the slurry at a constant speed in a concurrent flow manner within 80 minutes, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry2The mass is 1.0 percent, the pH value of the slurry is controlled to be 6.0, and the slurry is stirred and dispersed for 100 minutes;
5. filtering the obtained slurry by a 500-mesh screen, washing the slurry by deionized water or distilled water to obtain a filter cake, drying the filter cake, crushing the dried material, and simultaneously adding 75% of octyl phosphonic acid solution in a concurrent flow manner, wherein the addition amount of the octyl phosphonic acid solution is TiO calculated by phosphonic acid20.8 percent of the mass, and the crushed material is the titanium white chloride 5 special for the plastic color master batch.
Comparative example 3
The specific operation steps are as follows:
1. adding deionized water or distilled water into a pulping tank with a stirring device, starting stirring, and adding a modified polycarboxylate pulping dispersant into the pulping tank, wherein the addition amount of the modified polycarboxylate pulping dispersant is 0.25 percent of the content of titanium dioxide;
2. adding a titanium dioxide primary product by a chlorination process into a pulping tank, adding a certain amount of deionized water or distilled water, controlling the concentration of the slurry at 550g/L, and stirring and dispersing for 45 minutes;
3. transferring the pulped and dispersed pulp into a sand mill for grinding and depolymerization, and filtering the depolymerized pulp through a 500-mesh screen to obtain filtered pulp;
4. adding the filtered slurry into coating equipment with a stirring device, starting stirring, diluting the slurry to 250g/L by using deionized water or distilled water, heating and maintaining the system temperature at 65 ℃, adding an aluminum sulfate solution and 12% dilute alkali liquor into the slurry at a constant speed in a concurrent flow manner within 80 minutes, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated as TiO in the slurry2The mass is 1.0 percent, the pH value of the slurry is controlled to be 6.0, and the slurry is stirred and dispersed for 100 minutes;
5. filtering the obtained slurry by a 500-mesh screen, washing the slurry by deionized water or distilled water to obtain a filter cake, drying the filter cake, crushing the dried material, and simultaneously adding an organic silicon solution in a concurrent flow manner, wherein the addition amount of the organic silicon solution is TiO20.8 percent of the mass, and the crushed material is the titanium white chloride 6 special for the plastic color master batch.
The titanium dioxide obtained in the examples 1-3 and the comparative examples 1-3 is subjected to high-temperature volatile matter, dispersibility, hue and ultraviolet aging resistance tests, and the detection method comprises the following steps: weighing a certain amount of the titanium dioxide obtained in the examples 1-3 and the comparative examples 1-3, putting the titanium dioxide into an oven, measuring the volatile matters at 105 ℃ and 300 ℃, wherein the difference between the volatile matters at 300 ℃ and the volatile matters at 105 ℃ is the high-temperature volatile matter value, and the lower the value is, the better the high-temperature volatile matter is. The titanium dioxide obtained in the above examples 1-3 and comparative examples 1-3 was mixed with PP resin uniformly in a certain ratio, and the filter pressing value was measured by a filter pressing value tester, and the lower the filter pressing value, the better the dispersibility. The titanium dioxide obtained in the above examples 1 to 3 and comparative examples 1 to 3 was tabletted by a tabletting machine, and then the L value and the b value were measured by a color difference meter, and the higher the L value and the lower the b value, the better the hue was represented. The obtained plastic plate was irradiated with QUV, and the values of L, a and b before and after irradiation of the sample plate were measured with a color difference meter, and the color difference Δ E was calculated by the following formula, and the larger Δ E represents the poorer ultraviolet aging resistance of the sample plate.
Figure BDA0002651161310000071
The test results of the samples obtained in examples 1 to 3 and comparative examples 1 to 3 are shown in table 1 below.
TABLE 1 test results of samples obtained in examples 1 to 3 and comparative examples 1 to 3
Sample (I) High temperature volatile fraction/%) Dispersibility bar/g Value of L b value Color difference Δ E
Example 1 0.21 0.15 94.97 0.23 0.44
Example 2 0.24 0.18 94.71 0.38 0.46
Example 3 0.20 0.09 95.05 0.17 0.41
Comparative example 1 0.35 0.34 94.21 0.54 0.66
Comparative example 2 0.44 0.51 93.42 0.63 0.87
Comparative example 3 0.59 0.67 93.07 0.79 0.99
From the results of the examples and comparative examples, it can be seen that: by adopting the method, the high-temperature volatile matter of the prepared titanium dioxide is reduced, and the high-temperature resistance is better; the titanium pigment has better dispersibility and better ultraviolet aging resistance, can meet the special requirements of the field of plastic color masterbatch, provides special titanium pigment with better quality for the application field of plastic color masterbatch, and has important economic benefit.

Claims (10)

1. The preparation method of the titanium white chloride special for the plastic color master batch is characterized by comprising the following steps:
a. adding water into a pulping tank, and adding a pulping dispersant under the stirring condition, wherein the addition amount of the pulping dispersant is 0.1-0.5% of the content of titanium dioxide;
b. adding the titanium dioxide primary product by the chlorination process into a pulping tank, adding water until the concentration of the slurry is 300-800 g/L, and stirring and dispersing for 30-60 min;
c. b, transferring the slurry obtained in the step b into a sand mill for grinding and depolymerization, and filtering the depolymerized slurry through a screen with 200-800 meshes to obtain filtered slurry;
d. diluting the filtered slurry obtained in the step c to 200-300 g/L with water, heating and maintaining the system temperature at 50-80 ℃, adding dilute alkali liquor into the slurry at a constant speed within 50-150 min to adjust the pH value of the slurry to 5-7, and stirring and dispersing for 50-150 min;
e. d, adding an aluminum sulfate solution and a dilute alkali liquor into the slurry obtained in the step d at a constant speed in a parallel flow mode within 30-120 min, controlling the pH value of the slurry to be 5-7, stirring and dispersing for 50-150 min, and coating;
f. and e, filtering the slurry obtained in the step e by using a 200-800-mesh screen, washing to obtain a filter cake, drying and crushing the filter cake, and adding a phosphonic acid solution into the filter cake in a concurrent flow manner to obtain the titanium white special for the high-end plastic color master.
2. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: the pulping dispersing agent in the step a is modified polycarboxylate.
3. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: TiO in the titanium dioxide primary product by chlorination process in the step b2The content of (A) is more than or equal to 95 percent.
4. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: and c, grading the slurry obtained in the step c, wherein the particle size D50 of titanium dioxide particles in the graded slurry is 0.25-0.45 mu m, and D90 is less than or equal to 0.8 mu m.
5. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: the adding amount of the aluminum sulfate solution in the step d is Al2O3Measured as TiO in the slurry20.5 to 1.5% by mass.
6. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: and c, the volume concentration of the dilute alkali liquor in the step d is 8-15%.
7. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: and f, the content of phosphonic acid in the phosphonic acid solution is more than or equal to 70 percent.
8. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: and f, the phosphonic acid solution is an octyl phosphonic acid solution.
9. The preparation method of the titanium white chloride special for the plastic color masterbatch according to claim 1, characterized in that: the adding amount of the phosphonic acid solution in the step f is TiO20.3 to 1.5% by mass.
10. The titanium white chloride special for plastic color masterbatch prepared by the method of any one of claims 1-9.
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CN100564434C (en) * 2003-08-01 2009-12-02 千年无机化学公司 The inorganic solid particles that organic phosphine compound is handled
CN108603043A (en) * 2015-10-02 2018-09-28 亨茨曼P&A英国有限公司 Particle surface processing

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CN1123808A (en) * 1994-10-14 1996-06-05 泰奥塞集团服务有限公司 Treated titanium dioxide
US20040265348A1 (en) * 2003-06-05 2004-12-30 Jane Hollenberg Cosmetic compositions containing organophosphonic acid coated particulates and methods for producing the same
CN100564434C (en) * 2003-08-01 2009-12-02 千年无机化学公司 The inorganic solid particles that organic phosphine compound is handled
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