CN111019402A - Preparation method of high-weather-resistance titanium dioxide - Google Patents
Preparation method of high-weather-resistance titanium dioxide Download PDFInfo
- Publication number
- CN111019402A CN111019402A CN201911312294.0A CN201911312294A CN111019402A CN 111019402 A CN111019402 A CN 111019402A CN 201911312294 A CN201911312294 A CN 201911312294A CN 111019402 A CN111019402 A CN 111019402A
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- preparation
- coating
- weather resistance
- high weather
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 41
- 239000011248 coating agent Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 238000004537 pulping Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- URRHWTYOQNLUKY-UHFFFAOYSA-N [AlH3].[P] Chemical compound [AlH3].[P] URRHWTYOQNLUKY-UHFFFAOYSA-N 0.000 claims description 4
- DNXNYEBMOSARMM-UHFFFAOYSA-N alumane;zirconium Chemical compound [AlH3].[Zr] DNXNYEBMOSARMM-UHFFFAOYSA-N 0.000 claims description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 2
- 239000012756 surface treatment agent Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000004381 surface treatment Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 17
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
-
- 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
- C09C1/3607—Titanium dioxide
- C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C1/3623—Grinding
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
Abstract
The invention discloses a preparation method of high weather-resistant titanium dioxide, which comprises the steps of pulping titanium dioxide base materials, carrying out inorganic coating, sanding after coating, carrying out microwave hydrothermal reaction, washing with water, drying, and grinding with steam to obtain the high weather-resistant titanium dioxide. The preparation method of the super weather-resistant titanium dioxide adopts a special surface treatment process, and can form a more uniform and compact vitreous oxidation film layer on the surface of the titanium dioxide by the coating amount not exceeding 6wt% of the total mass of the titanium dioxide and the lower coating temperature; the product obtained by the invention not only has high weather resistance, but also has excellent dispersibility and storage stability, and has better formula applicability in downstream customers due to small coating amount.
Description
Technical Field
The invention relates to the field of titanium dioxide preparation, and particularly relates to a preparation method of high-weather-resistance titanium dioxide.
Background
Titanium dioxide is a very important white pigment, has wide application, can see the body shadow in all aspects of life, and is known as monosodium glutamate which is a chemical raw material and a weather meter of national economy.
Along with the improvement of living standard of people, the demand of the people on the aesthetic feeling around the living is more and more strict, such as the demand of automobile, ship anticorrosive paint and indoor and outdoor paint to keep bright and beautiful at any time and to resist the weather. And the weather resistance of the titanium dioxide is required to be higher.
In order to improve the weather resistance of titanium dioxide, titanium dioxide manufacturers mostly adopt a large amount of coating methods or a high-temperature calcination method to improve the weather resistance of titanium dioxide. Although the weather resistance of the titanium dioxide can be improved by a large amount of coating methods, the compactness of a film layer is not guaranteed, so that the titanium dioxide has larger oil absorption or water absorption, is only suitable for a high PVC pigment system, and limits the application field of the titanium dioxide. Although the weather resistance of titanium dioxide can be improved by reducing active groups on the surface of titanium dioxide through a high-temperature calcination manner, such as the patent with the patent number of US2671031, the titanium dioxide is sintered after the high-temperature calcination, and then needs to be sanded, so that the energy consumption is high, and a harder oxide layer is formed due to the fact that hydroxyl on the surface of the titanium dioxide is removed at high temperature, so that the grindability of the titanium dioxide is affected, and the compatibility with some resins is also reduced due to the loss of the hydroxyl on the surface, so that the application field of the titanium dioxide is affected.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of high-weather-resistance titanium dioxide.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a preparation method of high weather resistance titanium dioxide is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1, pulping titanium dioxide base materials, heating to 30-50 ℃, and performing inorganic coating to obtain coated slurry; the concentration of pulping is 180-320 g/L;
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 0.22-0.40 mu m;
step 3, transferring the ground slurry obtained in the step 2 into a hydrothermal reaction kettle in a microwave reaction furnace, and carrying out microwave hydrothermal reaction at the reaction temperature of 80-180 ℃ for 0.5-4 h to obtain reacted slurry;
and 4, cooling the reacted slurry obtained in the step 3, washing with water, drying, and performing vapor powder to obtain the high-weather-resistance titanium dioxide.
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 total coating amount of the inorganic coating in the step 1 is not more than TiO26wt% of the total mass; the inorganic coating 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:Al2O30.5-6 parts by weight of (= 1: 0.5-6); the zirconium-aluminum is coated with ZrO2With Al2O3In terms of mass ratio of ZrO2:Al2O31: 1-10; the phosphor-aluminum coating is coated with P2O5With Al2O3Meter with mass ratio of P2O5:Al2O3=1:1～8。
Preferably, the grain diameter of the sand grinding in the step 2 is controlled within the range of 0.28-0.35 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 treating agent is added in one of the drying and the steam powder in the step 4.
Preferably, the organic surface treatment agent is a polyhydric alcohol or an alcohol havingOne of organic silicon; the added organic surface treating agent accounts for TiO calculated as solute20.01 to 1 wt% of the total mass.
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 carries out low-amount inorganic coating on the titanium dioxide and then carries out a sanding working section. The sanding working section is adjusted from before coating to after coating, so that the inorganic coated film layer is recombined to form a more uniform film layer on the surface of the titanium dioxide, and then microwave hydrothermal treatment is carried out, so that the uniform film layer is further firmly combined to the surface of the titanium dioxide in a chemical bonding mode, and a complete, uniform and compact vitreous oxidation film layer is further formed, so that the titanium dioxide has excellent dispersibility, high weather resistance, better formula applicability and storage stability. And when the microwave hydrothermal reaction is carried out, the hydrothermal reaction time is 0.5-4 h, the reaction time is short, and the production efficiency is improved.
The invention adopts a special surface treatment process, uses lower coating amount (less than or equal to 6wt%, based on the total mass of the titanium dioxide) and lower coating temperature (30-50 ℃) and microwave hydrothermal reaction, and can form a more uniform and compact vitreous oxidation film layer on the surface of the titanium dioxide to achieve high weather resistance.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the super weather-resistant titanium dioxide adopts a special surface treatment process, and can form a more uniform and compact vitreous oxidation film layer on the surface of the titanium dioxide by the coating amount not exceeding 6wt% of the total mass of the titanium dioxide and the lower coating temperature; the product obtained by the invention not only has high weather resistance, but also has excellent dispersibility and storage stability, and has better formula applicability in downstream customers due to small coating amount.
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 paint formulation suitability data for each product from examples of the present invention and comparative examples;
FIG. 3 is data of storage stability test in formulation 1 for each product obtained in the examples of the present 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 to 180g/L, heating to 30 ℃, and adjusting the pH value to 10.2 by using a sodium hydroxide solution; adding sodium silicate Solution (SiO) with the total mass of 2.5wt percent of titanium dioxide2Metering), adding time is 30 min; adjusting pH of the slurry to 6.0 with dilute sulfuric acid for 120min, homogenizing for 30min, adding aluminum sulfate solution (Al) with 2.5wt% 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; carrying out microwave hydrothermal reaction at 150 ℃ for 1.5 h; cooling to 50 ℃, washing with water (the conductivity of the washing 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 0.35wt% of the total weight, and the steam-solid ratio is 1.8.
Example 2
Pulping qualified chlorination-process base materials, diluting to 220g/L, heating to 40 ℃, and adjusting the pH to 10.6 by using a sodium hydroxide solution; adding sodium silicate Solution (SiO) with the total mass of 2.0wt percent of titanium dioxide2Metering), adding time is 30 min; adjusting pH of the slurry to 6.0 with dilute sulfuric acid for 150min, homogenizing for 30min, adding aluminum sulfate solution (Al) with 3.0wt% 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 30min, and then sanding, wherein the grain size of the sanding is controlled to be 0.30 mu m; microwave water at 130 deg.CCarrying out thermal reaction for 0.5 h; cooling to 50 ℃, washing with water (the conductivity of the washing is less than 100 mu s/cm), flash evaporation and steam powder are carried out to obtain a product 2. Adding TiO in terms of solute during steam powder2TMP accounting for 0.35wt% of the total weight, and the steam-solid ratio is 1.8.
Example 3
Taking qualified chlorination process base materials, pulping and diluting to 280g/L, heating to 50 ℃, and adjusting the pH to 7.2 by using a sodium hydroxide solution; adding zirconium oxychloride solution (ZrO) with the total mass of 1.0wt% of titanium dioxide2Metering), adding time is 30 min; adjusting pH of the slurry to 8.5 with sodium hydroxide solution for 60min, homogenizing for 30min, adding aluminum sulfate solution (Al) 4.0wt% 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 30min, homogenizing for 30min, and then sanding, wherein the grain size of the sanding is controlled to be 0.29 mu m; carrying out microwave hydrothermal reaction at 80 ℃ for 4 h; cooling to 50 ℃, washing with water (the conductivity of the washing is less than 100 mu s/cm), flash evaporation and steam powder are carried out to obtain a product 3. Adding TiO in terms of solute during steam powder2TMP accounting for 0.35wt% of the total weight, and the steam-solid ratio is 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
Using example 1 as a reference, the chlorinated base material was sand-milled and then inorganic-coated, and the microwave hydrothermal reaction was replaced with calcination (calcination temperature 500 ℃ C., calcination time 3 hours), and the remaining steps were the same as in example 1, to obtain 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 the heavy coating and calcining processes 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
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 and dispersibility in the formula 1 and the formula 2, and has better formula applicability.
3. Storage stability in formulation 1
The paint prepared according to the formula 1 is used for carrying out storage stability test on the product 1, the product 2, the product 3, the comparative product 1 and the comparative product 2, and the test conditions and the judgment standard (the time is 30 days) are as follows:
and (3) putting the sample into a 50 ℃ oven, periodically testing the viscosity and the dispersity of the sample, and observing whether the sample has an obvious delamination phenomenon, wherein the delta viscosity of the sample is more than or equal to 500cp or the dispersity of the sample is more than or equal to 60 mu m or the sample has an obvious delamination phenomenon, so that the storage stability of the sample is not passed, otherwise, the sample passes.
As shown in FIG. 3, it can be seen that the titanium dioxide powder product prepared by the present invention has better storage stability, which is the storage stability test data of each product obtained in the examples and the comparative examples in the formula 1.
In conclusion, the titanium dioxide prepared by the invention has high weather resistance, excellent dispersibility, formula applicability and storage stability.
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 (8)
1. A preparation method of high weather resistance titanium dioxide is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step 1, pulping titanium dioxide base materials, heating to 30-50 ℃, and performing inorganic coating to obtain coated slurry; the concentration of pulping is 180-320 g/L;
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 0.22-0.40 mu m;
step 3, transferring the ground slurry obtained in the step 2 into a hydrothermal reaction kettle in a microwave reaction furnace, and carrying out microwave hydrothermal reaction at the reaction temperature of 80-180 ℃ for 0.5-4 h to obtain reacted slurry;
and 4, cooling the reacted slurry obtained in the step 3, washing with water, drying, and performing vapor powder to obtain the high-weather-resistance titanium dioxide.
2. The preparation method of high weather resistance titanium dioxide according to claim 1, which is characterized in that: 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 of high weather resistance titanium dioxide according to claim 1, which is characterized in that: the total coating amount of the inorganic coating in the step 1 is not more than TiO26wt% of the total mass; the inorganic coating is one of a silicon-aluminum coating, a zirconium-aluminum coating and a phosphorus-aluminum coating.
4. The preparation method of high weather resistance titanium dioxide according to claim 3, characterized in that: the siliconAluminum coated with SiO2With Al2O3Measured by mass ratio of SiO2:Al2O30.5-6 parts by weight of (= 1: 0.5-6); the zirconium-aluminum is coated with ZrO2With Al2O3In terms of mass ratio of ZrO2:Al2O31: 1-10; the phosphor-aluminum coating is coated with P2O5With Al2O3Meter with mass ratio of P2O5:Al2O3=1:1～8。
5. The preparation method of high weather resistance titanium dioxide according to claim 1, which is characterized in that: and the grain size of the sand grinding in the step 2 is controlled within the range of 0.28-0.35 mu m.
6. The preparation method of high weather resistance titanium dioxide according to claim 1, which is characterized in that: the sanding process of the step 2 adopts one of a vertical sand mill or a horizontal sand mill.
7. The preparation method of high weather resistance titanium dioxide according to claim 1, which is characterized in that: and (4) adding an organic surface treatment agent in one of the drying process and the steam-powder process in the step 4.
8. The preparation method of high weather resistance titanium dioxide according to claim 7, characterized in that: the organic surface treating agent 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911312294.0A CN111019402A (en) | 2019-12-18 | 2019-12-18 | Preparation method of high-weather-resistance titanium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911312294.0A CN111019402A (en) | 2019-12-18 | 2019-12-18 | Preparation method of high-weather-resistance titanium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111019402A true CN111019402A (en) | 2020-04-17 |
Family
ID=70210403
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911312294.0A Pending CN111019402A (en) | 2019-12-18 | 2019-12-18 | Preparation method of high-weather-resistance titanium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111019402A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621171A (en) * | 2020-05-22 | 2020-09-04 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN114591635A (en) * | 2022-03-04 | 2022-06-07 | 河南佰利联新材料有限公司 | Preparation method of high-weather-resistance high-gloss titanium dioxide |
| CN114874696A (en) * | 2021-06-25 | 2022-08-09 | 上海维巳达实业有限公司 | High-temperature-resistant paint for spray marking and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3767455A (en) * | 1970-01-15 | 1973-10-23 | Laporte Industries Ltd | Treatment of oxide pigments |
| CN101143978A (en) * | 2007-11-13 | 2008-03-19 | 攀枝花学院 | Composite envelope titanium white powder and preparation method thereof |
| CN110003687A (en) * | 2019-04-26 | 2019-07-12 | 龙蟒佰利联集团股份有限公司 | Preparation method of special titanium dioxide for high-gloss outdoor coating |
| 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 |
-
2019
- 2019-12-18 CN CN201911312294.0A patent/CN111019402A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3767455A (en) * | 1970-01-15 | 1973-10-23 | Laporte Industries Ltd | Treatment of oxide pigments |
| CN101143978A (en) * | 2007-11-13 | 2008-03-19 | 攀枝花学院 | Composite envelope titanium white powder and preparation method thereof |
| CN110003687A (en) * | 2019-04-26 | 2019-07-12 | 龙蟒佰利联集团股份有限公司 | Preparation method of special titanium dioxide for high-gloss outdoor coating |
| 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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621171A (en) * | 2020-05-22 | 2020-09-04 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN111621171B (en) * | 2020-05-22 | 2022-02-08 | 中信钛业股份有限公司 | Method for improving compactness of silicon dioxide coating layer on surface of titanium dioxide |
| CN114874696A (en) * | 2021-06-25 | 2022-08-09 | 上海维巳达实业有限公司 | High-temperature-resistant paint for spray marking and preparation method thereof |
| CN114874696B (en) * | 2021-06-25 | 2023-12-12 | 上海维巳达实业有限公司 | High-temperature-resistant paint for spray marks and preparation method thereof |
| CN114591635A (en) * | 2022-03-04 | 2022-06-07 | 河南佰利联新材料有限公司 | Preparation method of high-weather-resistance high-gloss titanium dioxide |
| CN114591635B (en) * | 2022-03-04 | 2023-08-11 | 河南佰利联新材料有限公司 | Preparation method of high-weather-resistance high-gloss titanium dioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111019402A (en) | Preparation method of high-weather-resistance titanium dioxide | |
| CN109705630B (en) | Preparation method of titanium dioxide pigment for high-light-resistance laminated paper | |
| CN110903681A (en) | Preparation method of super-weather-resistant titanium dioxide | |
| CN105670393B (en) | Cellulose nanocrystal body/silica composite shuttering method prepares super-hydrophobic coat | |
| US4125412A (en) | Process for the production of durable titanium dioxide pigment | |
| CN107163855B (en) | A kind of silica aerogel reflective insulation exterior wall paint and preparation method thereof | |
| CN110079129A (en) | A kind of preparation method of extra-weather-proof titanium dioxide | |
| CN104119703B (en) | A kind of preparation method of high gloss Rutile type Titanium Dioxide | |
| JPS62267370A (en) | Titanium pigment coated with cerium cation, selected acid anion and alumina | |
| CN113088105B (en) | High-weather-resistance titanium dioxide and preparation method thereof | |
| CN111234567B (en) | Inorganic coating process for preparing high-weather-resistance titanium dioxide | |
| CN105789339A (en) | Perovskite solar cell nano silicon dioxide coating liquid and application thereof | |
| CN110028812B (en) | Special preparation method for improving weather resistance of titanium dioxide | |
| CN111454592A (en) | Modified titanium dioxide and preparation method and application thereof | |
| CN110564182A (en) | surface treatment process of special titanium dioxide for high weather-resistant paint | |
| CN111057442A (en) | Preparation method of hollow mesoporous silica \ APS \ graphene oxide nano container | |
| CN109651848B (en) | Preparation method of special titanium dioxide for inner printing ink | |
| US9505022B2 (en) | Surface treatment method for making high durability universal titanium dioxide rutile pigment | |
| CN112480718B (en) | High-gloss high-weatherability titanium dioxide and preparation method thereof | |
| CN117070114B (en) | Quick rain-resistant weather-resistant water-based silicon-fluorine acrylic finish paint and preparation method thereof | |
| CN107955415A (en) | Lightfastness titanium dioxide and preparation method thereof, application | |
| CN110951282A (en) | Preparation method for improving weather resistance of titanium dioxide | |
| CN113372776B (en) | Building sun-proof heat-insulating coating and preparation method thereof | |
| CN111100482B (en) | Titanium suboxide black pigment and preparation method thereof | |
| CN107760133A (en) | A kind of preparation method of the organo-mineral complexing coating of nanometer of lanthanum hexaboride collaboration enhancing effect of heat insulation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200417 |
|
| RJ01 | Rejection of invention patent application after publication |