WO2022073390A1 - 一种高耐候锐钛型钛白粉制备方法 - Google Patents

一种高耐候锐钛型钛白粉制备方法 Download PDF

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WO2022073390A1
WO2022073390A1 PCT/CN2021/113454 CN2021113454W WO2022073390A1 WO 2022073390 A1 WO2022073390 A1 WO 2022073390A1 CN 2021113454 W CN2021113454 W CN 2021113454W WO 2022073390 A1 WO2022073390 A1 WO 2022073390A1
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titanium dioxide
anatase titanium
minutes
weather
resistant
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French (fr)
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张修臻
张本发
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安徽金星钛白（集团）有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
    • 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
    • C09C3/043—Drying, calcination
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • 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
    • C09C3/12—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
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62—L* (lightness axis)
    • 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
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
    • 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

Definitions

  • the invention belongs to the technical field of titanium dioxide production, and more particularly relates to a preparation method of high weather-resistant anatase titanium dioxide.
  • Weather resistance refers to the ability of products containing titanium dioxide pigments to be exposed to outdoor climates to resist the effects of sunlight and the atmosphere, and to avoid discoloration, chalking, and loss of light.
  • the photochemical activity of titanium dioxide pigment is the main factor affecting the weather resistance. Due to the existence of some lattice defects in titanium dioxide itself, there are many photoactivation points on its surface, which have slight absorption in the visible ultraviolet spectrum. Under the irradiation of ultraviolet light for a long time, if the With the action of catalysts such as water, titanium dioxide can undergo continuous redox reactions to generate hydroxyl and peroxy hydroxyl radicals. They are highly active and can oxidize organic polymers in products, resulting in polymer chain scission and degradation.
  • Chinese patent CN103496739A discloses a preparation method of weather-resistant titanium dioxide, which comprises doping metatitanic acid after bleaching and secondary water washing, and the doping method is as follows: Aqueous solutions of phosphorus compound, magnesium compound, antimony compound, aluminum compound, lithium compound, and potassium compound were sequentially added to the metatitanic acid after the secondary water washing, and the mixture was uniformly mixed.
  • Another example is Chinese patent CN109734126A, which discloses a method for preparing titanium dioxide with high weather resistance. The steps are as follows: a. Slurrying and dispersing metatitanic acid to prepare metatitanic acid slurry; b.
  • step d put the material into a heating furnace for heat treatment; e. when the temperature of the material in step d is When the temperature rises to 850 to 950 °C/min, the temperature is kept for 60 to 180 minutes. f. Cool the material obtained in step h to 0 to 35° C. within 1 to 20 minutes; g. pulverize the material obtained in step j and sieve it.
  • FIG. 1 Another example is Chinese patent CN110028812A, which discloses a special preparation method for improving the weather resistance of titanium dioxide, including the following steps: 1) preparing a titanium dioxide slurry, adding a silicate solution, and coating the first layer of silicon film; 2) coating the coating After the silicon film is applied, the pH value of the slurry is adjusted to 2-4, homogenized, and FeSO4 solution and dilute alkali solution are added at the same time, and the pH value of the slurry is maintained at 2-4, and then homogenized; 3) Add silicate again solution, coating the second layer of silicon film; 4) adding aluminum salt solution and dilute acid or dilute alkali solution at the same time, coating the aluminum film; 5) the slurry after coating the aluminum film is washed with water, flashed, and steamed to obtain Finished titanium dioxide.
  • Another example is Chinese patent CN110204928A, which discloses a method for producing high-weather-resistant titanium dioxide.
  • Chinese patent CN109096794A which discloses a preparation method of high weather-resistant titanium dioxide, including pulping, dispersion, silicate preparation, sand grinding, secondary sand grinding, silicate preparation, silicate preparation, aluminum salt preparation and
  • the inorganic acid in the steps S4, S6 and S7 is any one of dilute sulfuric acid, dilute phosphoric acid and dilute hydrochloric acid, and the concentration is 140-160 g/L.
  • Chinese patent CN105062150A which discloses a treatment method for improving the weather resistance of titanium dioxide.
  • the invention uses sodium silicate as raw material and adopts a two-step method to simultaneously realize the functions of dispersing agent and coating silica during the coating process of titanium dioxide.
  • Another example is Chinese patent CN103756367A, which discloses a preparation method of coated anatase titanium dioxide, slurrying, adding silicate aqueous solution, adding first soluble aluminum salt aqueous solution, adding sodium metaaluminate aqueous solution, adding the remaining second soluble aluminum Brine solution, add NaOH aqueous solution, filter and wash with 40-70 °C desalinated water until the resistivity of the filtrate is less than 100 ⁇ s/m, the material is dried and pulverized to obtain a titanium dioxide pigment sample.
  • the present invention provides a preparation method of the anatase titanium dioxide with high weather resistance, which can effectively improve the weather resistance of the anatase titanium dioxide.
  • the high-weather-resistant anatase titanium dioxide preparation method of the present invention comprises the following specific steps:
  • step S101 the filter cake after the second washing is transferred to a pulping tank for pulping, and the obtained slurry is transferred to a salt treatment tank;
  • step S102 the obtained slurry is diluted, heated up with steam, and subjected to inorganic surface treatment:
  • the obtained slurry is diluted to 220-250g/L with desalinated water, and heated to 80-90°C;
  • Step S103 transferring the clinker into a plate-and-frame filter press for three washings with desalinated water, and the end point is controlled at 200-300 ⁇ s cm, to obtain a filter cake after the three washings;
  • step S104 the filter cake after three washings is transferred to a rotary kiln for calcination, and the calcined crystal transformation temperature is controlled at 700-800 °C to obtain a crude anatase titanium dioxide;
  • step S105 the obtained crude anatase titanium dioxide is subjected to roller grinding to obtain powder with smaller particles, and D50 is 0.3-0.4 ⁇ m;
  • step S106 the titanium dioxide powder is transferred to a steam powder machine for organic coating, and at the same time, airflow pulverization is performed to obtain a finished titanium dioxide powder.
  • the solid content of the filter cake after the second washing is 35%-40%.
  • the mass concentration of the dilute phosphoric acid is 100-110 g/L, and the added amount is 0.2%-0.4% of P 2 O 5 in TiO 2 .
  • the mass concentration of the KOH solution is 15%-20%.
  • the concentration of SiO 2 in the sodium silicate solution is 90-110 g/L, and the addition amount is 10%-15% of SiO 2 in the TiO 2 .
  • the mass concentration of the dilute sulfuric acid is 120-130 g/L.
  • the Al 2 O 3 concentration content in the aluminum sulfate solution is 90-110 g/L, and the addition amount is 2%-3% of the Al 2 O 3 content in the TiO 2 .
  • the jet pulverization pressure is 1.5-2.0 MPa
  • the conveying pressure is 1.5-1.8 MPa
  • the organic coating agent can be selected from TMP, silicone or TME.
  • an inorganic coating is carried out before the preparation of the crude product is completed, and part of the process of the finished product of titanium dioxide is omitted. Phosphoric acid is dispersed, and then silicon coating is performed. In this process, sodium silicate is added for coating.
  • silica can enter the photoactive point during high temperature calcination, which greatly improves the weather resistance of titanium dioxide;
  • the weather resistance of anatase titanium dioxide is more dominant than that of conventional rutile titanium dioxide;
  • dilute phosphoric acid first plays a dispersing role, and can also act as a rutile inhibitor during calcination, reducing the tendency of titanium dioxide to rutile type.
  • Potassium hydroxide adjusts the pH to ensure that the pH before the addition of sodium silicate is neutral; the function of dilute sulfuric acid is to adjust the pH and stabilize the pH before the salt treatment;
  • the calcined crystal transformation temperature is controlled at 700-800° C., and the obtained titanium dioxide is anatase titanium dioxide;
  • the unit consumption of white powder natural gas is low, which effectively reduces the cost; in addition, the anatase titanium dioxide powder is soft and easy to crush;
  • the mass concentration of dilute phosphoric acid is 100-110g/L, and the added amount is 0.2%-0.4% (calculated as P 2 O 5 ), and phosphoric acid plays a dispersing role, mainly It is to reduce the viscosity of the slurry and ensure the coating effect in the later stage.
  • Fig. 1 is the flow chart of the preparation method of high-weather-resistant anatase titanium dioxide of the present invention.
  • the flow chart of the preparation method of high weather-resistant anatase titanium dioxide of the present invention wherein the chemicals include dilute phosphoric acid, potassium hydroxide solution, sodium silicate solution, dilute sulfuric acid and aluminum sulfate solution.
  • the solid content of the filter cake after the second wash is 35%-40%;
  • the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 220-250g/L with desalinated water, and heated to 80-90°C; (2) Add dilute phosphoric acid solution while stirring, preferably, the mass concentration of the dilute phosphoric acid is 100-110g/L, the amount added is 0.2%-0.4% of P 2 O 5 in the TiO 2 , and it is aged for 30 minutes; (3) Add KOH solution while stirring to adjust the pH to 7.5-8.0, preferably, the mass concentration of the KOH solution is 15%-20%, and mature for 30 minutes; (4) add sodium silicate solution while stirring, preferably, the described In the sodium silicate solution, the concentration of SiO 2 is 90-110 g/L, the amount of SiO 2 coating is 10%-15%, and it is aged for 60 minutes; (5) adding dilute sulfuric acid while stirring, preferably, the quality of the dilute
  • the jet crushing pressure is 1.5-2.0 MPa
  • the conveying pressure is 1.5-1.8 MPa
  • the organic coating agent can be selected from TMP, silicone or TME, and the jet crushing is carried out at the same time.
  • the finished product of titanium dioxide is obtained.
  • the inorganic coating is carried out before the preparation of the crude product is completed, and part of the process of the finished product of titanium dioxide is omitted. After that, the silicon coating is carried out. In this process, sodium silicate is added to carry out the coating. After calcination, the silica can enter the photoactive point during the high temperature calcination process, which greatly improves the weather resistance of titanium dioxide;
  • the inventor of the present invention found that the calcined sodium silicate has extremely high weather resistance through a large number of tests and analysis, and the calcination can reduce the temperature to generate anatase titanium dioxide, and the calcination temperature is lower than the calcination temperature of rutile titanium dioxide, The energy consumption will be reduced.
  • the possible reason is that sodium silicate is heated to decompose sodium oxide and silicon dioxide, and the melting point of sodium oxide is low, thereby reducing the calcination temperature; silicon dioxide can enter the photoactive point during high temperature calcination, which greatly improves titanium dioxide.
  • dilute phosphoric acid first plays a dispersing role, and can also play a role as a rutile inhibitor during calcination, reducing the conversion of titanium dioxide to rutile type; potassium hydroxide Adjust the pH to make sure that the pH before the addition of sodium silicate is neutral; the function of dilute sulfuric acid is also to adjust the pH to stabilize the pH before the salt treatment.
  • the specific steps are as follows: transfer the filter cake after the second washing into a pulping tank for pulping, and transfer the prepared slurry into a salt treatment tank; The solid content of the filter cake after washing is 40%; the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 250 g/L with desalinated water, and heated to 90 ° C; (2) ) while stirring, add a dilute phosphoric acid solution with a mass concentration of 110 g/L, the dosage is 0.4% in terms of P 2 O 5 , and ripen for 30 minutes; (3) while stirring, add a KOH solution with a mass concentration of 15% to adjust the pH to 8.0, ripening for 30 minutes; (4) adding SiO while stirring the sodium silicate solution that the concentration content is 110g/L, the SiO coating amount is 15 %, and ripening for 60 minutes; (5) adding the mass
  • the jet pulverization pressure is 2.0 MPa
  • the conveying pressure is 1.8 MPa
  • the organic coating is carried out.
  • TMP is selected as the agent, and the finished product of titanium dioxide is obtained by jet pulverization at the same time.
  • the specific steps are as follows: transfer the filter cake after the second washing into a pulping tank for pulping, and transfer the prepared slurry into a salt treatment tank; The solid content of the filter cake after washing is 35%; the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 220 g/L with desalinated water, and heated to 80 ° C; (2) ) while stirring, add a dilute phosphoric acid solution with a mass concentration of 100 g/L, the dosage is 0.2% in terms of P 2 O 5 , and mature for 30 minutes; (3) while stirring, add a KOH solution with a mass concentration of 15% to adjust the pH to 7.5, ripening for 30 minutes; (4) adding SiO while stirring The sodium silicate solution with a concentration content of 90 g/L, SiO The coating amount is 10%, and ripening for 60 minutes; (5) adding the mass
  • the crude titanium dioxide is subjected to roller mill grinding to obtain powder with smaller particles; the titanium dioxide powder is transferred to a steam pulverizer for organic coating. Silicone is selected as the coating agent, and the finished titanium dioxide is obtained by jet pulverization at the same time.
  • the specific steps are as follows: transfer the filter cake after the second washing into a pulping tank for pulping, and transfer the prepared slurry into a salt treatment tank; The solid content of the filter cake after washing is 38%; the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 240 g/L with desalinated water, and heated to 85 ° C; (2) ) while stirring, add a dilute phosphoric acid solution with a mass concentration of 105 g/L, the dosage is 0.3% in terms of P 2 O 5 , and mature for 30 minutes; (3) adding a KOH solution with a mass concentration of 20% while stirring to adjust the pH to 7.5, ripening for 30 minutes; (4) adding SiO while stirring The sodium silicate solution with a concentration content of 100 g /L, the SiO coating amount is 14%, and ripening for 60 minutes; (5) adding
  • the crude titanium dioxide is subjected to roller mill grinding to obtain powder with smaller particles; the titanium dioxide powder is transferred to a steam pulverizer for organic coating.
  • the coating agent is TME, and the finished product of titanium dioxide is obtained by jet pulverization at the same time.
  • the specific steps are as follows: transfer the filter cake after the second washing into a pulping tank for pulping, and transfer the prepared slurry into a salt treatment tank; The solid content of the filter cake after washing is 38%; the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 240 g/L with desalinated water, and heated to 85 ° C; (2) ) while stirring, add a dilute phosphoric acid solution with a mass concentration of 100 g/L, the dosage is 0.4% in terms of P 2 O 5 , and mature for 30 minutes; (3) while stirring, add a KOH solution with a mass concentration of 16% to adjust the pH to 7.5, ripening for 30 minutes; (4) adding SiO while stirring the sodium silicate solution with a concentration content of 110 g/L, the SiO coating amount is 12 %, and ripening for 60 minutes; (5)
  • the specific steps are as follows: transfer the filter cake after the second washing into a pulping tank for pulping, and transfer the prepared slurry into a salt treatment tank; The solid content of the filter cake after washing is 40%; the obtained slurry is diluted, steamed and matured, and inorganic surface treated: (1) the obtained slurry is diluted to 230 g/L with desalinated water, and heated to 90 ° C; (2) ) while stirring, add a dilute phosphoric acid solution with a mass concentration of 100 g/L, the dosage is 0.25% in terms of P 2 O 5 , and ripen for 30 minutes; (3) while stirring, add a KOH solution with a mass concentration of 17% to adjust the pH to 7.5, ripening for 30 minutes; (4) adding SiO while stirring the sodium silicate solution that the concentration content is 105g/L, the SiO coating amount is 14 %, and ripening for 60 minutes;
  • the airflow pulverization pressure is 1.5MPa, and the conveying pressure is 1.6MPa , Organic silicon is selected as the organic coating agent, and the finished product of titanium dioxide is obtained by jet pulverization at the same time.
  • Anatase titanium dioxide has great advantages in L value and b value.
  • the goal of titanium dioxide industry is to improve the whiteness (L value) of titanium dioxide and reduce b value as much as possible to obtain blue-phase titanium dioxide.
  • L value whiteness
  • rutile The calcination temperature of titanium dioxide is relatively high, and it generally has a yellow phase; in addition, the calcination temperature of this titanium dioxide is relatively low, which can effectively reduce the unit consumption of natural gas, and this titanium dioxide does not need to go through most of the post-treatment processes, and it is not necessary for equipment, auxiliary materials, manpower, environmental protection The cost of other aspects has also been effectively controlled.

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Abstract

本发明公开了一种高耐候锐钛型钛白粉制备方法，属于钛白粉生产技术领域。该方法通过在二洗后滤饼制浆后的偏钛酸进行无机包膜，经过无机包膜后的浆料进行洗涤、煅烧得到钛白粉粗品，钛白粉粗品经过辊压磨研磨，研磨后的钛白粉经过气流粉碎工序进行有机包膜，得到高耐候锐钛型钛白粉。本发明的高耐候锐钛型钛白粉制备方法，在粗品制备完成之前进行无机包膜，省掉钛白粉成品部分工序，优点是：在二洗后的滤饼经过制浆，用磷酸进行分散，之后进行硅包膜，在这个工序加入硅酸钠进行包膜经过煅烧后，二氧化硅在高温煅烧过程能进入光活性点，极大提高钛白粉的耐候性。

Description

一种高耐候锐钛型钛白粉制备方法 技术领域
本发明属于钛白粉生产技术领域，更具体地说，涉及一种高耐候锐钛型钛白粉制备方法。
背景技术
耐候性是指含有二氧化钛颜料的制品暴露在室外气候环境下，抵抗日光和大气的作用，避免发生变色、粉化、失光的能力。二氧化钛颜料的光化学活性是影响耐候性的主要因素，由于二氧化钛本身存在一些晶格缺陷，其表面上存在许多光活化点，对可见光紫外光谱段有轻微的吸收，长期在紫外光的照射下，如果有水等催化剂的作用，钛白粉可发生连续的氧化还原反应，生成羟基和过氧羟基自由基，它们具有高度的活性，能使制品中的有机聚合物氧化，发生高分子链断链和降解，破坏制品的连续性，使制品的耐候性降低。因此，需要通控制偏钛酸的煅烧制度、控制其冷却速度、均匀晶粒、增加内应力、钉扎氧空位、抑制电子移动，降低其光化学作用的破坏力，从而提高制品耐候性。
为了解决上述的问题，经检索，例如中国专利CN103496739A公开了一种耐候性钛白粉的制备方法，该方法包括对经过漂白、二次水洗后的偏钛酸进行掺杂，所述掺杂方法为向二次水洗后的偏钛酸中依次加入磷化合物、镁化合物、锑化合物、铝化合物、锂化合物、钾化合物的水溶液，混合均匀。再如中国专利CN109734126A公开了一种高耐候性钛白粉的制备方法，其步骤如下：a、将偏钛酸打浆分散处理，制得偏钛酸浆料；b、将浆料中依次加入煅烧晶种、钾化合物、磷化合物、铝化合物，搅拌30～90min；c、将浆料放入烘箱进行烘干；d、将物料放入加热炉中进行加热处理；e、当步骤d中的物料温度升至850～950℃/min时，保温60～180min。f、将步骤h获得的物料，在1～20min内冷却到0～35℃；g、将步骤j获得的物料进行粉碎，并筛分。再如中国专利CN110028812A公开了一种特殊的提高钛白粉耐候性的制备方法，包括以下步骤：1)制备钛白粉料浆，加入硅酸盐溶液，包覆第一层硅膜；2)将包覆硅膜后料浆的pH值调节为2-4，均化，同时加入FeSO4溶液和稀碱溶液，并维持料浆的pH值为2-4，然后均化；3)再加入硅酸盐溶液，包覆第二层硅膜；4)同时加入铝盐溶液和稀酸或稀碱溶液，包覆铝膜；5)包覆铝膜后的料浆经水洗、闪蒸、汽粉，得到钛白粉成品。再如中国专利CN110204928A公开了一种高耐候钛白粉生产方法，首先，制备二氧化钛含量为250-400g/L的初始浆液，然后再在特定的条件下，通过多次包膜工艺，对二氧化钛进行钛、硅、磷、铝等包膜，并严格控制各每次包膜的工艺条件，包覆均匀，有效提高钛白粉的耐候性能，改善其颜料性能。再如中国专利CN109096794A公开了一种高耐候钛白粉的制备方法，包括制浆，分散，硅酸盐调制、砂磨，二次砂磨，硅酸盐调制，硅酸盐调制，铝 盐调制及干燥和粉碎等八个步骤，所述的S4、S6、S7步骤中无机酸为稀硫酸、稀磷酸及稀盐酸中的任意一种，浓度为140-160g/L。再如中国专利CN105062150A公开了一种提高钛白粉耐候性的处理方法。本发明在钛白粉进行无机表面处理的过程中，利用硅酸钠为原料，采用两步法，在二氧化钛包膜过程中同时实现分散剂和包覆二氧化硅的功能。再如中国专利CN103756367A公开了一种包膜锐钛型钛白粉的制备方法，制浆，加入硅酸盐水溶液，加入第一可溶性铝盐水溶液，加入偏铝酸钠水溶液，加入余下第二可溶性铝盐水溶液，加入NaOH水溶液，用40-70℃脱盐水进行过滤洗涤至滤液电阻率小于100μs/m，物料经干燥、粉碎处理，制得二氧化钛颜料样品。
上述公开的文献均是对耐候性钛白粉不断改进，但是，这些方案均有待改善，从而提高锐钛型钛白粉的性能。
发明内容
1.要解决的问题
针对现有锐钛型钛白粉的耐候性不能满足使用要求的问题，本发明提供一种高耐候锐钛型钛白粉制备方法，有效地提高锐钛型钛白粉的耐候性。
2.技术方案
为了解决上述问题，本发明所采用的技术方案如下：
本发明的高耐候锐钛型钛白粉制备方法，其具体步骤为：
步骤S101、将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽；
步骤S102、得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：
(1)得到的浆料用脱盐水进行稀释至220-250g/L，升温至80-90℃；
(2)边搅拌边加入稀磷酸溶液，熟化30分钟；
(3)边搅拌边加入KOH溶液调pH至7.5-8.0，熟化30分钟；
(4)边搅拌边加入硅酸钠溶液，熟化60分钟；
(5)边搅拌边加入稀硫酸，调pH至7.0-7.5，熟化30分钟；
(6)边搅拌边并流加入硫酸铝溶液和KOH溶液，确保pH在6.0-7.0之间，熟化60分钟；
(7)调整pH在6.0-6.5，熟化30分钟，得到熟料；
步骤S103、将熟料转入板框压滤机用脱盐水进行三洗，终点控制在200-300μs·cm，得到三洗后的滤饼；
步骤S104、三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在700-800℃，得到锐钛型钛白粉粗品；
步骤S105、得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末，D50在0.3-0.4μm；
步骤S106、钛白粉粉末转入汽粉机进行有机包膜，同时进行气流粉碎得到钛白粉成品。
于本发明一种可能实施方式中，所述二洗后的滤饼固含量在35％-40％。
于本发明一种可能实施方式中，所述稀磷酸质量浓度为100-110g/L，加入量为TiO 2中以P 2O 5含量为0.2％-0.4％。
于本发明一种可能实施方式中，所述KOH溶液质量浓度为15％-20％。
于本发明一种可能实施方式中，所述硅酸钠溶液中SiO 2浓度含量为90-110g/L，加入量为TiO 2中以SiO 2含量为10％-15％。
于本发明一种可能实施方式中，所述稀硫酸质量浓度为120-130g/L。
于本发明一种可能实施方式中，所述硫酸铝溶液中Al 2O 3浓度含量为90-110g/L，加入量为TiO 2中以Al 2O 3含量为2％-3％。
于本发明一种可能实施方式中，所述气流粉碎工序中，气流粉碎压力为1.5-2.0MPa，输送压力为1.5-1.8MPa，有机包膜剂可以选择TMP、有机硅或TME。
3.有益效果
相比于现有技术，本发明的有益效果为：
(1)本发明的高耐候锐钛型钛白粉制备方法，在粗品制备完成之前进行无机包膜，省掉钛白粉成品部分工序，优点是：在二洗后的滤饼经过制浆，用稀磷酸进行分散，之后进行硅包膜，在这个工序加入硅酸钠进行包膜经过煅烧后，二氧化硅在高温煅烧过程能进入光活性点，极大提高钛白粉的耐候性；二氧化硅提高了锐钛型钛白粉的耐候性，相比常规金红石型钛白粉更占优势；另外说明，稀磷酸首先起分散作用，在煅烧时又可以起到金红石抑制剂的作用，减少钛白粉向金红石型的转化；氢氧化钾调节pH，确定硅酸钠加入前的pH处于中性；稀硫酸的作用是可以调pH，稳定盐处理前的pH；
(2)本发明的高耐候锐钛型钛白粉制备方法，煅烧的晶型转化温度控制在700-800℃，得到的钛白粉为锐钛型钛白粉；该方法的煅烧温度较低，此钛白粉天然气单耗较低，有效降低成本；另外，锐钛型钛白粉质较软，易粉碎；
(3)本发明的高耐候锐钛型钛白粉制备方法，稀磷酸质量浓度为100-110g/L，加量在0.2％-0.4％(以P 2O 5计)，磷酸起分散作用，主要是降低浆料粘度，确保后期包膜效果。
附图说明
图1为本发明高耐候锐钛型钛白粉制备方法的流程图。
具体实施方式
下文对本发明的示例性实施例进行了详细描述。尽管这些示例性实施例被充分详细地描述以使得本领域技术人员能够实施本发明，但应当理解可实现其他实施例且可在不脱离本发明的精神和范围的情况下对本发明作各种改变。下文对本发明的实施例的更详细的描述并不用于限制所要求的本发明的范围，而仅仅为了进行举例说明且不限制对本发明的特点和特征的描述，以提出执行本发明的最佳方式，并足以使得本领域技术人员能够实施本发明。因此，本发明的范围仅由所附权利要求来限定。
下文对本发明的详细描述和示例实施例进行说明。
如图1所示，本发明高耐候锐钛型钛白粉制备方法的流程图，其中化学品包括稀磷酸、氢氧化钾溶液、硅酸钠溶液、稀硫酸和硫酸铝溶液。将矿物经酸解、沉降过滤、结晶除绿矾、浓缩得浓钛液，再进行水解、一次水洗得到一洗偏钛酸浆料；将一洗偏钛酸浆料进行漂白；将漂白后的偏钛酸进行二次水洗；将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，优选的，所述二洗后的滤饼固含量在35％-40％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至220-250g/L，升温至80-90℃；(2)边搅拌边加入稀磷酸溶液，优选的，所述稀磷酸质量浓度为100-110g/L，加入量为TiO 2中以P 2O 5含量为0.2％-0.4％，熟化30分钟；(3)边搅拌边加入KOH溶液调pH至7.5-8.0，优选的，所述KOH溶液质量浓度为15％-20％，熟化30分钟；(4)边搅拌边加入硅酸钠溶液，优选的，所述硅酸钠溶液中SiO 2浓度含量为90-110g/L，SiO 2包膜量为10％-15％，熟化60分钟；(5)边搅拌边加入稀硫酸，优选的，所述稀硫酸质量浓度为120-130g/L，调pH至7.0-7.5，熟化30分钟；(6)边搅拌边并流加入硫酸铝溶液和KOH溶液，优选的，所述硫酸铝溶液中Al 2O 3浓度含量为90-110g/L，加入量为TiO 2中以Al 2O 3含量为2％-3％，确保pH在6.0-7.0之间，熟化60分钟；(7)调整pH在6.0-6.5，熟化30分钟，得到熟料；将熟料转入板框压滤机用脱盐水进行三洗，终点控制在200-300μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在700-800℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为1.5-2.0MPa，输送压力为1.5-1.8MPa，有机包膜剂可以选择TMP、有机硅或TME，同时进行气流粉碎得到钛白粉成品。
本发明的高耐候锐钛型钛白粉制备方法，在粗品制备完成之前进行无机包膜，省掉钛白粉成品部分工序，优点是：在二洗后的滤饼经过制浆，用磷酸进行分散，之后进行硅包膜，在这个工序加入硅酸钠进行包膜经过煅烧后，二氧化硅在高温煅烧过程能进入光活性点，极大提高钛白粉的耐候性；
本发明的发明人通过大量的试验和分析，发现经过煅烧的硅酸钠具有极高的耐候性，且 煅烧可以降低温度生成锐钛型钛白粉，煅烧温度低于金红石型钛白粉的煅烧温度，能耗会降低，可能的原因是硅酸钠受热分解氧化钠和二氧化硅，氧化钠的熔点低，从而降低煅烧温度；二氧化硅在高温煅烧过程能进入光活性点，极大提高钛白粉的耐候性；相比常规金红石型钛白粉更占优势；另外说明，稀磷酸首先起分散作用，在煅烧时又可以起到金红石抑制剂的作用，减少钛白粉向金红石型的转化；氢氧化钾调节pH，确定硅酸钠加入前的pH处于中性；稀硫酸的作用也是调pH，稳定盐处理前的pH。
实施例1
本实施例的高耐候锐钛型钛白粉制备方法，其具体步骤为：将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，所述二洗后的滤饼固含量在40％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至250g/L，升温至90℃；(2)边搅拌边加入质量浓度为110g/L的稀磷酸溶液，加量以P 2O 5计在0.4％，熟化30分钟；(3)边搅拌边加入质量浓度为15％的KOH溶液调pH至8.0，熟化30分钟；(4)边搅拌边加入SiO 2浓度含量为110g/L的硅酸钠溶液，SiO 2包膜量为15％，熟化60分钟；(5)边搅拌边加入质量浓度为120g/L的稀硫酸，调pH至7.5，熟化30分钟；(6)边搅拌边并流加入Al 2O 3浓度含量为110g/L的硫酸铝溶液和KOH溶液，Al 2O 3包膜量为2％，确保pH在7.0，熟化60分钟；(7)调整pH在6.5，熟化30分钟，得到熟料；将熟料转入板框压滤机用脱盐水进行三洗，终点控制在300μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在800℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为2.0MPa，输送压力为1.8MPa，有机包膜剂选择TMP，同时进行气流粉碎得到钛白粉成品。
实施例2
本实施例的高耐候锐钛型钛白粉制备方法，其具体步骤为：将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，所述二洗后的滤饼固含量在35％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至220g/L，升温至80℃；(2)边搅拌边加入质量浓度为100g/L的稀磷酸溶液，加量以P 2O 5计在0.2％，熟化30分钟；(3)边搅拌边加入质量浓度为15％的KOH溶液调pH至7.5，熟化30分钟；(4)边搅拌边加入SiO 2浓度含量为90g/L的硅酸钠溶液，SiO 2包膜量为10％，熟化60分钟；(5)边搅拌边加入质量浓度为130g/L的稀硫酸，调pH至7.5，熟化30分钟；(6)边搅拌边并流加入Al 2O 3浓度含量为90g/L的硫酸铝溶液和KOH溶液，Al 2O 3包膜量为3％，确保pH在7.0之间，熟化60分钟；(7)调整pH在6.0，熟化30分钟，得到熟料；将熟料转入板框压滤机 用脱盐水进行三洗，终点控制在200μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在700℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为1.5MPa，输送压力为1.5MPa，有机包膜剂选择有机硅，同时进行气流粉碎得到钛白粉成品。
实施例3
本实施例的高耐候锐钛型钛白粉制备方法，其具体步骤为：将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，所述二洗后的滤饼固含量在38％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至240g/L，升温至85℃；(2)边搅拌边加入质量浓度为105g/L的稀磷酸溶液，加量以P 2O 5计在0.3％，熟化30分钟；(3)边搅拌边加入质量浓度为20％的KOH溶液调pH至7.5，熟化30分钟；(4)边搅拌边加入SiO 2浓度含量为100g/L的硅酸钠溶液，SiO 2包膜量为14％，熟化60分钟；(5)边搅拌边加入质量浓度为125g/L的稀硫酸，调pH至7.5，熟化30分钟；(6)边搅拌边并流加入Al 2O 3浓度含量为100g/L的硫酸铝溶液和KOH溶液，Al 2O 3包膜量为3％，确保pH在6.5之间，熟化60分钟；(7)调整pH在6.5，熟化30分钟，得到熟料；将熟料转入板框压滤机用脱盐水进行三洗，终点控制在250μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在750℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为1.8MPa，输送压力为1.6MPa，有机包膜剂选择TME，同时进行气流粉碎得到钛白粉成品。
实施例4
本实施例的高耐候锐钛型钛白粉制备方法，其具体步骤为：将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，所述二洗后的滤饼固含量在38％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至240g/L，升温至85℃；(2)边搅拌边加入质量浓度为100g/L的稀磷酸溶液，加量以P 2O 5计在0.4％，熟化30分钟；(3)边搅拌边加入质量浓度为16％的KOH溶液调pH至7.5，熟化30分钟；(4)边搅拌边加入SiO 2浓度含量为110g/L的硅酸钠溶液，SiO 2包膜量为12％，熟化60分钟；(5)边搅拌边加入质量浓度为120g/L的稀硫酸，调pH至7.5，熟化30分钟；(6)边搅拌边并流加入Al 2O 3浓度含量为110g/L的硫酸铝溶液和KOH溶液，Al 2O 3包膜量为2％，确保pH在7.0之间，熟化60分钟；(7)调整pH在6.5，熟化30分钟，得到熟料；将熟料转入板框压滤机用脱盐水进行三洗，终点控制在280μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行 煅烧，煅烧的晶型转化温度控制在780℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为1.8MPa，输送压力为1.5MPa，有机包膜剂选择TMP，同时进行气流粉碎得到钛白粉成品。
实施例5
本实施例的高耐候锐钛型钛白粉制备方法，其具体步骤为：将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽，所述二洗后的滤饼固含量在40％；得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：(1)得到的浆料用脱盐水进行稀释至230g/L，升温至90℃；(2)边搅拌边加入质量浓度为100g/L的稀磷酸溶液，加量以P 2O 5计在0.25％，熟化30分钟；(3)边搅拌边加入质量浓度为17％的KOH溶液调pH至7.5，熟化30分钟；(4)边搅拌边加入SiO 2浓度含量为105g/L的硅酸钠溶液，SiO 2包膜量为14％，熟化60分钟；(5)边搅拌边加入质量浓度为125g/L的稀硫酸，调pH至7.0，熟化30分钟；(6)边搅拌边并流加入Al 2O 3浓度含量为90-110g/L的硫酸铝溶液和KOH溶液，Al 2O 3包膜量为3％，确保pH在6.0之间，熟化60分钟；(7)调整pH在6.0，熟化30分钟，得到熟料；将熟料转入板框压滤机用脱盐水进行三洗，终点控制在220μs·cm，得到三洗后的滤饼；三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在720℃，得到锐钛型钛白粉粗品；得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末；钛白粉粉末转入汽粉机进行有机包膜，所述气流粉碎工序中，气流粉碎压力为1.5MPa，输送压力为1.6MPa，有机包膜剂选择有机硅，同时进行气流粉碎得到钛白粉成品。
下面给出本发明实施例1至5锐钛型钛白粉测试结果。
  L(％) b值 消色力 耐候性(ΔE) 分散性(μm)
对比样 95.41 1.94 1980 0.45 25
实施例1 95.69 1.35 1890 0.33 25
实施例2 95.78 1.31 1880 0.30 22.5
实施例3 95.72 1.42 1890 0.33 25
实施例4 95.77 1.43 1880 0.29 22.5
实施例5 95.79 1.38 1870 0.25 25
综述：锐钛型钛白粉在L值、b值存在很大优势，目前钛白粉行业目标是尽量提高钛白粉的白度(L值)、降低b值，得到蓝相的钛白粉，但是由于金红石钛白粉煅烧温度较高，其一般呈黄相；另外，本钛白粉煅烧温度较低，有效降低天然气单耗，并且本钛白粉不用经过后处理大部分工序，在设备、辅材、人力、环保等方面的成本也得到了有效的控制。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (8)

  1. 一种高耐候锐钛型钛白粉制备方法，其特征在于，其具体步骤为：
    步骤S101、将二洗后的滤饼转入制浆槽进行制浆，所制得的浆料转入盐处理槽；
    步骤S102、得到的浆料进行稀释、蒸汽升温熟化、无机表面处理：
    (1)得到的浆料用脱盐水进行稀释至220-250g/L，升温至80-90℃；
    (2)边搅拌边加入稀磷酸溶液，熟化30分钟；
    (3)边搅拌边加入KOH溶液调pH至7.5-8.0，熟化30分钟；
    (4)边搅拌边加入硅酸钠溶液，熟化60分钟；
    (5)边搅拌边加入稀硫酸，调pH至7.0-7.5，熟化30分钟；
    (6)边搅拌边并流加入硫酸铝溶液和KOH溶液，确保pH在6.0-7.0之间，熟化60分钟；
    (7)调整pH在6.0-6.5，熟化30分钟，得到熟料；
    步骤S103、将熟料转入板框压滤机用脱盐水进行三洗，终点控制在200-300μs·cm，得到三洗后的滤饼；
    步骤S104、三洗后的滤饼转入转窑进行煅烧，煅烧的晶型转化温度控制在700-800℃，得到锐钛型钛白粉粗品；
    步骤S105、得到的锐钛型钛白粉粗品进行辊压磨研磨，得到颗粒较小的粉末，D50在0.3-0.4μm；
    步骤S106、钛白粉粉末转入汽粉机进行有机包膜，同时进行气流粉碎得到钛白粉成品。
  2. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述二洗后的滤饼固含量在35％-40％。
  3. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述稀磷酸质量浓度为100-110g/L，加入量为TiO 2中以P 2O 5含量为0.2％-0.4％。
  4. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述KOH溶液质量浓度为15％-20％。
  5. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述硅酸钠溶液中SiO 2浓度含量为90-110g/L，加入量为TiO 2中以SiO 2含量为10％-15％。
  6. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述稀硫酸质量浓度为120-130g/L。
  7. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述硫酸铝溶液中Al 2O 3浓度含量为90-110g/L，加入量为TiO 2中以Al 2O 3含量为2％-3％。
  8. 根据权利要求书1所述的高耐候锐钛型钛白粉的制备方法，其特征在于，所述气流粉 碎工序中，气流粉碎压力为1.5-2.0MPa，输送压力为1.5-1.8MPa，有机包膜剂可以选择TMP、有机硅或TME。
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