CN110951282A - Preparation method for improving weather resistance of titanium dioxide - Google Patents

Preparation method for improving weather resistance of titanium dioxide Download PDF

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Publication number
CN110951282A
CN110951282A CN201911310595.XA CN201911310595A CN110951282A CN 110951282 A CN110951282 A CN 110951282A CN 201911310595 A CN201911310595 A CN 201911310595A CN 110951282 A CN110951282 A CN 110951282A
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titanium dioxide
preparation
weather resistance
improving
steps
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陈建立
王永珊
冯亚阳
宋运萍
郭永阳
张健
司小锋
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Lomon Billions Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3615Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3653Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a preparation method for improving weather resistance of titanium dioxide. The invention adopts a special preparation method, and can form a more uniform and compact film layer on the surface of the titanium dioxide by coating the titanium dioxide with a coating amount not exceeding 5wt% of the total mass of the titanium dioxide and a lower coating temperature without prolonging the coating time; the product has high weather resistance, excellent dispersivity and good formula applicability.

Description

Preparation method for improving weather resistance of titanium dioxide
Technical Field
The invention relates to the field of titanium dioxide preparation, and particularly relates to a preparation method for improving weather resistance of titanium dioxide.
Background
Titanium dioxide is a very important white pigment and is widely applied to the industries of paint, printing ink, plastics, rubber, papermaking, chemical fiber and the like. Wherein the largest amount of the paint is 60 wt%, and in the paint, the percentage of the titanium dioxide in the building paint is 60 wt%. With the saturation of the architectural coating market, more and more downstream customers shift the eyes to industrial coatings, which are mostly outdoor coatings, and this puts higher requirements on the weather resistance of titanium dioxide.
Titanium dioxide has certain photocatalytic performance, so in order to improve the weather resistance of titanium dioxide, the photocatalytic performance of titanium dioxide needs to be reduced. Most titanium dioxide manufacturers at home and abroad usually adopt a large amount of coating methods to block photochemical active points of the titanium dioxide so as to reduce the photocatalytic performance of the titanium dioxide and improve the weather resistance of the titanium dioxide; a secondary coating method is also adopted to improve the weather resistance of the titanium dioxide. Although the weather resistance of the titanium dioxide can be improved, the oil absorption and water absorption of the obtained product are generally high, which affects the viscosity of the product in a downstream customer formula system and further affects the formula applicability of the product, thereby limiting the application field of the product. While the method adopting the secondary coating, such as the patent with the patent number of US3251705, can improve the weather resistance of the titanium dioxide, the secondary coating is carried out after the first coating is washed and dried for 15-20 h, the operation time is longer, and the product yield is not high.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method for improving the weather resistance of titanium dioxide.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a preparation method for improving the weather resistance of titanium dioxide comprises the following steps,
step 1, taking titanium dioxide base material and beatingPulping to obtain slurry; placing the slurry into a microwave reaction furnace, heating to 40-60 ℃, and then carrying out inorganic coating to obtain coated slurry; the coating amount of the inorganic coating is not more than TiO25wt% of the total mass;
step 2, sanding the coated slurry obtained in the step 1 to obtain sanded slurry; the grain size of the sand grinding is controlled within the range of 0.25-0.40 mu m;
step 3, washing, drying and steam-pulverizing the sand grinding slurry obtained in the step 2 to obtain a titanium dioxide product; adding an organic surface treating agent in one of the two processes of drying and steam-powder.
Preferably, the titanium dioxide base material in the step 1 is one of a chlorination-process base material or a sulfuric-process base material.
Preferably, the power of the microwave reaction furnace in the step 1 is 200-1800W.
Preferably, the power of the microwave reaction furnace in the step 1 is 800-1500W.
Preferably, the inorganic coating in step 1 is one of a silicon-aluminum coating, a zirconium-aluminum coating, and a phosphorus-aluminum coating.
Preferably, the silicon-aluminum coating is made of SiO2With Al2O3Measured by mass ratio of SiO2:Al2O3=1: 0.5-7; the zirconium-aluminum is coated with ZrO2With Al2O3In terms of mass ratio of ZrO2:Al2O31: 1-9; the phosphor-aluminum coating is coated with P2O5With Al2O3Meter with mass ratio of P2O5:Al2O3=1:1~10。
Preferably, the grain diameter of the sand grinding in the step 2 is controlled within the range of 0.29-0.34 μm.
Preferably, the sanding process of step 2 is one of a vertical type sanding machine and a horizontal type sanding machine.
Preferably, the organic surface treatment agent in step 3 is one of polyalcohol or organosilicon; the added organic surface treating agent accounts for TiO calculated as solute20.01 to 1 wt% of the total mass.
Preferably, the concentration of the beating in the step 1 is 200 g/L-300 g/L.
The titanium dioxide base materials used for pulping are all qualified titanium dioxide base materials; the processes of washing, drying and steam powder are all general processes of titanium dioxide production process.
The invention has the following function principle:
the invention adopts a microwave coating method, namely directly coats the titanium dioxide in a microwave reaction furnace, so that the bonding of the coating material and hydroxyl on the surface of the titanium dioxide is accelerated at a lower coating temperature, and a thin, uniform and compact vitreous oxidation film layer is formed on the surface of the titanium dioxide, thereby improving the weather resistance of the titanium dioxide.
According to the invention, after the sanding section is adjusted to be coated, the inorganic coated film layer can be recombined, so that a more complete, uniform and compact vitreous oxidation film layer is formed on the surface of the titanium dioxide, and the dispersibility, the formula applicability and the weather resistance of the titanium dioxide are further improved.
The invention adopts a special surface treatment process, uses lower coating amount (the coating amount is less than or equal to 5wt percent based on the total mass of the titanium dioxide) and lower coating temperature, and in the coating process, the coating time is maintained in the original operation time, the operation time in the coating process is not prolonged, so that a more uniform and compact vitreous oxidation film is formed on the surface of the titanium dioxide, and better formula applicability and high weather resistance are achieved.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a special preparation method, and can form a more uniform and compact film layer on the surface of the titanium dioxide by coating the titanium dioxide with a coating amount not exceeding 5wt% of the total mass of the titanium dioxide and a lower coating temperature without prolonging the coating time; the product has high weather resistance, excellent dispersivity and good formula applicability.
Drawings
FIG. 1 shows the results of a xenon lamp rapid aging test of each product obtained in examples and comparative examples of the present invention;
FIG. 2 is a graph of paint formulation suitability data for each product obtained in examples of the invention and comparative examples.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
Taking qualified chlorination process base materials, pulping and diluting the base materials into 280g/L, placing the base materials into a microwave reaction furnace, adjusting the microwave power to 1000W, heating to 60 ℃, and adjusting the pH value to 9.8 by using a sodium hydroxide solution; adding sodium silicate Solution (SiO) with the total mass of 2.2wt percent of titanium dioxide2Metering), adding time is 30 min; adjusting pH of the slurry to 6.2 with dilute sulfuric acid for 90min, homogenizing for 30min, adding aluminum sulfate solution (Al) with 2.3wt% of total mass of titanium dioxide2O3Metering), adding sodium hydroxide solution at the same time, keeping the pH value of the slurry to be 7.0, adding for 30min, homogenizing for 50min, and then sanding, wherein the grain size of the sanding is controlled to be 0.32 mu m; washing with water (the washing conductivity is less than 100 mu s/cm), flash evaporation and steam powder are carried out to obtain the product 1. Adding TiO in terms of solute during steam powder2TMP accounting for 0.45 weight percent of the total mass and the steam-solid ratio of 1.8.
Example 2
Taking qualified base materials of a chlorination method, pulping and diluting the base materials into 250g/L, placing the base materials into a microwave reaction furnace, adjusting the microwave power to 1200W, heating to 50 ℃, and adjusting the pH value to 11.2 by using a sodium hydroxide solution; adding sodium silicate Solution (SiO) with the total mass of titanium dioxide of 1.8wt%2Metering), adding time is 20 min; adjusting pH of the slurry to 6.3 with dilute sulfuric acid for 90min, homogenizing for 30min, adding aluminum sulfate solution (Al) with 2.7wt% of total mass of titanium dioxide2O3Metering), adding sodium hydroxide solution at the same time, keeping the pH value of the slurry to be 7.0, adding for 20min, homogenizing for 30min, and then sanding, wherein the grain size of the sanding is controlled to be 0.30 mu m; washing with water (the washing conductivity is less than 100 mu s/cm), flash evaporating, and steam pulverizing to obtain product 2. Adding TiO in terms of solute during steam powder2TMP accounting for 0.45 weight percent of the total mass and the steam-solid ratio of 1.8.
Example 3
Pulping qualified chlorination-process base materials to be diluted to 220g/L, placing the base materials into a microwave reaction furnace, adjusting the microwave power to 1400W, heating to 40 ℃, and adjusting the pH to 7.0 by using a sodium hydroxide solution; adding zirconium oxychloride solution (ZrO) with the total mass of 1.0wt% of titanium dioxide2Metering), adding time is 20 min; adjusting pH of the slurry to 8.7 with sodium hydroxide solution for 60min, homogenizing for 30min, adding aluminum sulfate solution (Al) 3.5wt% of total weight of titanium white2O3Metering), adding sodium hydroxide solution at the same time, keeping the pH value of the slurry to be 7.0, adding for 20min, homogenizing for 30min, and then sanding, wherein the grain size of the sanding is controlled to be 0.33 μm; washing with water (the washing conductivity is less than 100 mu s/cm), flash evaporating, and steam pulverizing to obtain product 3. Adding TiO in terms of solute during steam powder2TMP accounting for 0.40 weight percent of the total mass and the steam-solid ratio of 1.8.
Comparative example 1
Based on example 1, the chlorination process base material is first sanded and then inorganic coated, wherein the silicon coating accounts for 4wt% of the total weight of the titanium dioxide (SiO is used as a coating)2Calculated by the formula), the aluminum coating accounts for 6wt% (calculated as Al) of the total mass of the titanium dioxide2O3Meter). Then washing with water (the washing conductivity is less than 100 mu s/cm), flash evaporation and steam powder are carried out to obtain a comparative product 1. The amount of the auxiliary agent added in the steam powder is the same as that in example 1.
Comparative example 2
Taking the example 1 as a reference, sanding the chlorination process base material and then performing inorganic coating, wherein the inorganic coating process comprises the steps of firstly performing primary silicon-aluminum coating (half of coating amount), washing, drying at 120 ℃ for 18 hours, and then performing secondary silicon-aluminum coating; the remaining procedure was identical to that of example 1, giving comparative product 2.
The products obtained in the examples and the comparative examples are compared by application performance experiments
1. Xenon lamp rapid aging experiment
The xenon lamp rapid aging test was performed on the product 1, the product 2, the product 3, the comparative product 1, and the comparative product 2, and the test results were shown in fig. 1, in which the 60 ° light retention (%) was measured as a function of time.
As can be seen from FIG. 1, the titanium dioxide product prepared by the invention can achieve the weather resistance of the high-weather-resistance titanium dioxide prepared by heavy coating and secondary coating with less coating amount and lower coating temperature, and the titanium dioxide prepared by the invention has high weather resistance.
2. Comparison of coating formulation suitability
Figure DEST_PATH_IMAGE001
As shown in the above table, titanium dioxide is required to be added to both formulas 1 and 2 of the existing coating, the coating is prepared according to the formulas 1 and 2 for the product 1, the product 2, the product 3, the comparative product 1 and the comparative product 2, respectively, and the viscosity and the dispersibility of the coating are tested.
FIG. 2 shows the paint formulation suitability data for each product obtained in the examples and comparative examples. Compared with the comparative examples, the titanium dioxide product prepared by the invention has lower viscosity, better dispersibility and better formula applicability in the formula 1 and the formula 2.
In conclusion, the titanium dioxide prepared by the process method has high weather resistance, excellent dispersibility and better formula applicability.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.

Claims (10)

1. A preparation method for improving the weather resistance of titanium dioxide is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1, taking a titanium dioxide base material, and pulping to obtain slurry; placing the slurry into a microwave reaction furnace, heating to 40-60 ℃, and then carrying out inorganic coating to obtain coated slurry; the coating amount of the inorganic coating is not more than TiO25wt% of the total mass;
step 2, sanding the coated slurry obtained in the step 1 to obtain sanded slurry; the grain size of the sand grinding is controlled within the range of 0.25-0.40 mu m;
step 3, washing, drying and steam-pulverizing the sand grinding slurry obtained in the step 2 to obtain a titanium dioxide product; adding an organic surface treating agent in one of the two processes of drying and steam-powder.
2. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the titanium dioxide base material in the step 1 is one of a chlorination process base material or a sulfuric acid process base material.
3. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the power of the microwave reaction furnace in the step 1 is 200-1800W.
4. The preparation method for improving the weather resistance of titanium dioxide according to claim 3, wherein the preparation method comprises the following steps:
the power of the microwave reaction furnace in the step 1 is 800-1500W.
5. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps:
the inorganic coating in the step 1 is one of a silicon-aluminum coating, a zirconium-aluminum coating and a phosphorus-aluminum coating.
6. The preparation method for improving the weather resistance of titanium dioxide according to claim 5, wherein the preparation method comprises the following steps: the silicon-aluminum coating is made of SiO2With Al2O3Measured by mass ratio of SiO2:Al2O3=1: 0.5-7; the zirconium-aluminum is coated with ZrO2With Al2O3In terms of mass ratio of ZrO2:Al2O31: 1-9; the phosphor-aluminum coating is coated with P2O5With Al2O3Meter with mass ratio of P2O5:Al2O3=1:1~10。
7. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the grain size of the sand grinding in the step 2 is controlled within the range of 0.29-0.34 mu m.
8. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the sanding process of the step 2 adopts one of a vertical sand mill or a horizontal sand mill.
9. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the organic surface treating agent in the step 3 is one of polyalcohol or organic silicon; the added organic surface treating agent accounts for TiO calculated as solute20.01 to 1 wt% of the total mass.
10. The preparation method for improving the weather resistance of titanium dioxide according to claim 1, wherein the preparation method comprises the following steps: the concentration of the pulping in the step 1 is 200 g/L-300 g/L.
CN201911310595.XA 2019-12-18 2019-12-18 Preparation method for improving weather resistance of titanium dioxide Pending CN110951282A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113549344A (en) * 2021-06-29 2021-10-26 龙佰四川钛业有限公司 Titanium dioxide barium sulfate coating method

Citations (6)

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Publication number Priority date Publication date Assignee Title
CN1826387A (en) * 2003-06-17 2006-08-30 西巴特殊化学品控股有限公司 A process for the preparation of a pigment comprising a core material and at least one dielectric layer
CN102015913A (en) * 2008-04-25 2011-04-13 3M创新有限公司 Process for the surface modification of particles
CN104610877A (en) * 2013-11-01 2015-05-13 信越化学工业株式会社 Titania-containing coating composition and coated article
CN108864769A (en) * 2018-08-15 2018-11-23 龙蟒佰利联集团股份有限公司 A kind of preparation method of superelevation dispersibility slurry titanium white and titanium dioxide
CN109401365A (en) * 2017-08-18 2019-03-01 龙蟒佰利联集团股份有限公司 A kind of preparation method of inner-printing ink special titanium pigment
CN110079129A (en) * 2019-05-31 2019-08-02 龙蟒佰利联集团股份有限公司 A kind of preparation method of extra-weather-proof titanium dioxide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1826387A (en) * 2003-06-17 2006-08-30 西巴特殊化学品控股有限公司 A process for the preparation of a pigment comprising a core material and at least one dielectric layer
CN102015913A (en) * 2008-04-25 2011-04-13 3M创新有限公司 Process for the surface modification of particles
CN104610877A (en) * 2013-11-01 2015-05-13 信越化学工业株式会社 Titania-containing coating composition and coated article
CN109401365A (en) * 2017-08-18 2019-03-01 龙蟒佰利联集团股份有限公司 A kind of preparation method of inner-printing ink special titanium pigment
CN108864769A (en) * 2018-08-15 2018-11-23 龙蟒佰利联集团股份有限公司 A kind of preparation method of superelevation dispersibility slurry titanium white and titanium dioxide
CN110079129A (en) * 2019-05-31 2019-08-02 龙蟒佰利联集团股份有限公司 A kind of preparation method of extra-weather-proof titanium dioxide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113549344A (en) * 2021-06-29 2021-10-26 龙佰四川钛业有限公司 Titanium dioxide barium sulfate coating method

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