CN104925843A - Method for preparing laminar alpha-Al2O3 pearlescent pigment base material by use of compound aluminum salt - Google Patents

Method for preparing laminar alpha-Al2O3 pearlescent pigment base material by use of compound aluminum salt Download PDF

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CN104925843A
CN104925843A CN201510300413.6A CN201510300413A CN104925843A CN 104925843 A CN104925843 A CN 104925843A CN 201510300413 A CN201510300413 A CN 201510300413A CN 104925843 A CN104925843 A CN 104925843A
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sheet
salt
water soluble
soluble compound
compound aluminium
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王毅
李磊
祁光霞
袁超
雷雪飞
徐辉
孙应龙
尹丽丹
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Tsinghua University
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Tsinghua University
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Abstract

The invention discloses a method for preparing a laminar alpha-Al2O3 pearlescent pigment base material by use of compound aluminum salt. The compound aluminum salt (aluminium potassium sulfate or aluminum sodium sulfate) is selected as the aluminium source, and is hydrolyzed to produce a required fused salt in situ; under the condition of adding laminar alpha-Al2O3 seed crystals and crystal growth regulators (a titanium salt and a phosphate), a gel produced by reaction is dried and calcined at 850-1100 DEG C to prepare laminar alpha-Al2O3 with favorable properties, so that the method is simple in process. The obtained laminar alumina (0.2-0.5 [mu]m in average thickness, 11-15 [mu]m in average particle diameter, larger than 20 in diameter-to-thickness ratio and no clustering or crystal twinning) can serve as the pearlescent pigment base material.

Description

Clad aluminum salt is utilized to prepare laminar α-Al 2o 3the method of pearly pigment base material
Technical field
The invention belongs to Material Field, relate to one and utilize clad aluminum salt to prepare laminar α-Al 2o 3the method of pearly pigment base material.
Background technology
Natural mica owing to occurring that radius-thickness ratio is uneven containing impurity and cause traditional mica titanium nacreous material existing defects in the pearly-lustre such as color, colorimetric purity performance after grinding, and the flat substrates of synthetic (as platelet shaped iron oxide, laminar titanium oxide, flake aluminum oxide) becomes the new study hotspot of pearly pigment base material owing to having high refractive index.Especially, laminar α-Al 2o 3due to the desirable base material of advantage the becomes high-quality pearly pigment such as the crystal morphology of high-melting-point, high rigidity, high stability and building-up process, radius-thickness ratio be controlled, prepare the laminar α-Al of high-quality further by coated metal oxide (as titanium oxide) 2o 3based pearlescent pigments.
Synthetic flake α-Al 2o 3the method of pearly pigment base material mainly comprises molten-salt growth method, hydro-thermal (alcohol heat) method, high-temperature sintering process and mechanical process.Due to α-Al 2o 3fusing point is up to 2054 DEG C and physical strength is high, makes high-temperature sintering process and mechanical process etc. all cannot obtain the suitable laminar α-Al of size 2o 3; Hydrothermal method and the hot method of alcohol all make alpha-alumina crystals cleavage under the critical condition of water or alcohol dissolve by High Temperature High Pressure, and under the effect of crystal growth modifier, recrystallization generates sheet α-Al simultaneously 2o 3(Japanese Patent Laid-Open 3-131517, Unexamined Patent 7-331110, US Patent No. 0043910), but the sheet α-Al prepared 2o 3particle diameter and radius-thickness ratio are all less, easily form twin, are not suitable for use in pearly pigment base material, and high-temperature and high-pressure conditions needs expensive high-pressure reactor; Molten-salt growth method synthesizes laminar α-Al 2o 3be adopt one or several low melting point salts as reaction medium, reduce the growth transition activation energy of alpha-alumina crystals, alpha-alumina crystals is laminar α-Al through the effect anisotropic growth of crystal growth modifier 2o 3.Because liquid fused salt is α-Al 2o 3crystal growth provides an excellent chemical reaction place, therefore the laminar α-Al for preparing of molten-salt growth method 2o 3even particle size distribution, radius-thickness ratio is large, can be used as the base material of high-quality pearly pigment, possesses through engineering approaches application prospect.But, the simple inorganic aluminate of the large more options of method that the domestic patent of invention (CN 1150165A, CN 101541681A, CN 1936114A and CN 101660204A) related to adopts is as aluminium source, as Tai-Ace S 150, and need extra interpolation potassium sulfate and sodium sulfate mixture as additional fused-salt medium, one in titanyl sulfate, tin sulphate, zinc sulfate and sodium phosphate or two kinds are crystal growth modifier, then high-temperature calcination, flow process is comparatively complicated, the sheet α-Al prepared 2o 3character is very different, the laminar α-Al that high-temperature calcination obtains 2o 3character meets the condition as pearly pigment base material substantially, and adds powder α-Al 2o 3α-the Al that crystal seed obtains through 700 DEG C of calcinings 2o 3grain diameter is less, can not be used as pearly pigment base material.In sum, current laminar α-Al 2o 3preparation method all need additional a large amount of fused salt, both raw materials cost was increased, make again preparation flow complicated, calcining temperature is mostly 900-1200 DEG C, energy consumption is higher, and it is little through calcining the tabular alumina particle diameter obtained again simply to add Powdered crystal seed, the requirement as pearly pigment base material can not be met.
Summary of the invention
The object of this invention is to provide one utilizes clad aluminum salt to prepare laminar α-Al 2o 3the method of pearly pigment base material.
Preparation sheet α-Al provided by the invention 2o 3method, comprise the steps:
1) in the saturated aqueous solution of Water Soluble Compound aluminium salt, add crystal growth modifier, mixing obtains suspension liquid a;
2) in the aqueous solution of carbonate, Na is added 3pO 412H 2o, mixing obtains solution b;
3) when Keep agitation, by step 2) gained solution b joins step 1) in gained suspension liquid a, be hydrolyzed reaction, and react complete and dried by gained gel mixture, last calcining of pulverizing, obtains described sheet α-Al 2o 3.
The step 1 of aforesaid method) in, Water Soluble Compound aluminium salt is selected from least one in 12 hydrazine aluminum sulfate potassium and sodium alum;
Described crystal growth modifier is water-soluble titanium salt;
Described water-soluble titanium salt is specifically selected from least one in titanyl sulfate and titanium tetrachloride;
The add-on of described crystal growth modifier and the mol ratio of described Water Soluble Compound aluminium salt are 1:50-1:300, specifically can be 1:300,1:150 or 1:50.
Described step 2) in, carbonate is selected from least one in sodium carbonate and salt of wormwood;
The add-on of described carbonate is step 1) described in amount needed for Water Soluble Compound aluminium salt loading aqueous solution complete hydrolysis, namely the mol ratio of carbonate and Water Soluble Compound aluminium salt is 3:2;
Described Na 3pO 412H 2the add-on of O and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 1:70-1:280, specifically can be 1:280,1:140 or 1:70.
Described step 3) in hydrolysis reaction step, temperature is room temperature, and the time is 0.5 hour-2 hours, specifically can be 1 hour;
In described grinding steps, after grinding, the particle diameter of powder is 100 μm-200 μm;
In described calcining step, temperature is 1000-1100 DEG C, specifically can be 1000 DEG C or 1100 DEG C;
Time is 3 hours-7 hours, specifically can be 3 hours, 5 hours or 7 hours.
Described method also comprises the steps: in described step 3) after calcining step, by gained solid product through hot water dissolving, filter, washing, dry.
Present invention also offers another kind of preparation sheet α-Al 2o 3method, the method comprises the steps:
1) in the saturated aqueous solution of Water Soluble Compound aluminium salt, add crystal growth modifier and crystal seed, mixing obtains suspension liquid a;
Wherein, described crystal seed is aforementioned sheet α-Al provided by the invention 2o 3;
2) in the aqueous solution of carbonate, Na is added 3pO 412H 2o, mixing obtains solution b;
3) when Keep agitation, by step 2) gained solution b joins step 1) in gained suspension liquid a, be hydrolyzed reaction, and react complete and dried by gained gel mixture, last calcining of pulverizing, obtains described sheet α-Al 2o 3.
The step 1 of aforesaid method) in, Water Soluble Compound aluminium salt is selected from least one in 12 hydrazine aluminum sulfate potassium and sodium alum;
Described crystal growth modifier is water-soluble titanium salt;
Described water-soluble titanium salt is specifically selected from least one in titanyl sulfate and titanium tetrachloride;
The mol ratio of described crystal growth modifier and described Water Soluble Compound aluminium salt is 1:50-1:300, specifically can be 1:300,1:150 or 1:50;
Described sheet α-Al 2o 3the mol ratio of crystal seed and described Water Soluble Compound aluminium salt is 1:40-1:200, specifically can be 1:200,1:70 or 1:40;
Described step 2) in, carbonate is selected from least one in sodium carbonate and salt of wormwood;
The add-on of described carbonate is step 1) described in amount needed for Water Soluble Compound aluminium salt loading aqueous solution complete hydrolysis, namely the mol ratio of carbonate and Water Soluble Compound aluminium salt is 3:2;
Described Na 3pO 412H 2the add-on of O and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 1:70-1:280, specifically can be 1:280,1:140 or 1:70.
Described step 3) in hydrolysis reaction step, temperature is room temperature, and the time is 0.5 hour-2 hours, specifically can be 1 hour;
In described grinding steps, after grinding, the particle diameter of powder is 100 μm-200 μm;
In described calcining step, temperature is 850 DEG C-1100 DEG C, specifically can be 850 DEG C, 900 DEG C, 1000 DEG C or 1100 DEG C;
Time is 3 hours-7 hours, specifically can be 3 hours, 5 hours or 7 hours.
Described method also comprises the steps: in described step 3) after calcining step, by gained solid product through hot water dissolving, filter, washing, dry.
The technical process of above-mentioned two methods as shown in Figure 1.
In addition, according to the sheet α-Al that above-mentioned two methods prepare 2o 3and this sheet α-Al 2o 3in the application prepared in pearly pigment and with this sheet α-Al 2o 3for the pearly pigment of base material, also belong to protection scope of the present invention.Wherein, described sheet α-Al 2o 3mean thickness be 0.2 μm-0.5 μm, specifically can be 0.2 μm, 0.3 μm; Median size is 11 μm-13 μm or 11 μm-15 μm, specifically can be 11 μm, 12 μm, 13 μm, 14 μm, 15 μm; Radius-thickness ratio >20, specifically can be 47,50,55,60,47-65 or 65.
The present invention is directed to existing laminar α-Al 2o 3molten-salt growth method preparation technology needs additional a large amount of fused salt to increase raw materials cost, and flow process is comparatively complicated, and calcining temperature is higher causes the problems such as energy consumption is comparatively large, and the tabular alumina particle diameter that the Powdered crystal seed of simple interpolation obtains is little, provides the laminar α-Al of preparation 2o 3novel method.The method selects potassium aluminium sulfate or aluminium sodium sulfate, under interpolation salt of wormwood or sodium carbonate condition, through hydrolysis reaction, generate aluminum hydroxide gel and the sodium sulfate or the potassium sulfate that are adsorbed in gel surface simultaneously, above-mentioned vitriol plays the effect of fused salt in the subsequent calcination stage, then adds laminar α-Al 2o 3crystal seed and titanium salt, this gel mixture obtains the laminar α-Al of good properties through 850-1100 DEG C of calcining, washing and drying 2o 3, can be used as pearly pigment base material.
Sheet α-Al is prepared with existing molten-salt growth method 2o 3pearly pigment substrate process is compared, and beneficial effect of the present invention is as follows:
(1) the method belongs to molten-salt growth method but without the need to additional fused salt, and clad aluminum salt, as while aluminium source, generates required fused salt at hydrolysing step situ and is also adsorbed on aluminium hydroxide gel surface, both reduced raw materials cost, simultaneously simple flow;
(2) the laminar α-Al added 2o 3crystal seed significantly reduces follow-up sheet α-Al on the one hand 2o 3change and growth temperature, calcination temperature range is 850-1100 DEG C, and lowest calcination temperatures can be 850 DEG C, reduces energy consumption, can also promote sheet α-Al simultaneously 2o 3the growth of crystal.Laminar α-the Al prepared 2o 3good properties, meets the requirement as pearly pigment base material.Laminar α-the Al that the present invention is finally obtained 2o 3a part turns back in preparation flow as crystal seed, and crystal seed is conveniently easy to get.
Accompanying drawing explanation
Fig. 1 is that clad aluminum salt low-temperature simple prepares laminar α-Al 2o 3the process flow sheet of pearly pigment base material.
Fig. 2 is laminar α-Al in embodiment 1 2o 3scanning electron microscope (SEM) photograph, X ray diffracting spectrum and grain size distribution curve.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.
Embodiment 1
1) by 46.5g KAl (SO 4) 212H 2o is dissolved in 150mL deionized water, obtains KAl (SO 4) 212H 2the saturated aqueous solution of O, then add 0.11gTiOSO 4(purity 93%) or 3.7gTiCl 4the aqueous solution (mass percentage concentration is 3.2%), after it dissolves, fully stir 30min, obtained suspension liquid a;
2) by 15.6g anhydrous Na 2cO 3with 0.27g Na 3pO 412H 2o is dissolved in 150mL deionized water, obtained solution b;
3) to be joined by solution b in suspension liquid a and fully stir and to be hydrolyzed reaction in room temperature, reaction times 1h, obtains gel mixture after completion of the reaction.Above-mentioned gel mixture is dried in evaporation, dried gel abrasive become powder and cross 100 mesh standard sieves (< 150 μm), powder after being ground by gained calcines 5h at 1100 DEG C, obtain crystallization block, treat that temperature is cooled to room temperature, above-mentioned crystallization block is placed in boiling water dissolve, filters, wash and dry insoluble white solid, obtain laminar α-Al provided by the invention 2o 3.
This laminar α-Al 2o 3thickness is at 0.2 μm-0.5 μm, and median size is 11 μm and is evenly distributed, and radius-thickness ratio is greater than 20, without twin and reunion.
Embodiment 2
1) by 46.5g KAl (SO 4) 212H 2o is dissolved in 150mL deionized water, obtain KAl (SO 4) 212H 2the saturated aqueous solution of O, adds 0.11gTiOSO 4(purity 93%) or 3.7gTiCl 4the aqueous solution (mass percentage concentration is 3.2%), after it dissolves, then add 0.25g sheet α-Al 2o 3as crystal seed, fully stir 30min, obtained suspension liquid a; This step be used as the sheet α-Al of crystal seed 2o 3crystal seed is embodiment 1 products obtained therefrom;
2) by 15.6g anhydrous Na 2cO 3with 0.13g Na 3pO 412H 2o is dissolved in 150mL deionized water, obtained solution b;
3) to be joined by solution b in suspension liquid a and fully stir and to be hydrolyzed reaction in room temperature, reaction times 1h, obtains gel mixture after completion of the reaction.Above-mentioned gel mixture is dried in evaporation, dried gel abrasive become powder and cross 100 mesh standard sieves (< 150 μm), make particle diameter after 100 μm-200 μm, powder after being ground by gained calcines 5h at 1000 DEG C, obtain crystallization block, treat that temperature is cooled to room temperature, above-mentioned crystallization block is placed in boiling water and dissolves, filter, wash and dry insoluble white solid, obtain laminar α-Al provided by the invention 2o 3.
This laminar α-Al 2o 3x ray diffracting spectrum see Fig. 2.As seen from the figure, α-Al is only had in this product 2o 3the peak of (corundum).
Scanning electron microscopy picture and grain size distribution curve (see Fig. 2) show its thickness at 0.2 μm-0.5 μm, and particle diameter is at 4-40 μm, and median size is 12 μm and is evenly distributed, and radius-thickness ratio is greater than 20, without twin and reunion, when by this laminar α-Al 2o 3be added to the water and dispersed with stirring, can produce smooth streamline, this is the mark of good distribution.
Embodiment 3-8
The method of embodiment 3-8 is similar to embodiment 2, and difference is that the amount of additive is different, and detailed conditions is as described in Table 1.Gained flake α-Al 2o 3feature as shown in table 2.
Table 1, embodiment 1-8 experiment condition
In table 1, titanium source/aluminium source (mol ratio) is also the molar ratio of crystal growth modifier and Water Soluble Compound aluminium salt;
Na 3pO 412H 2o/ aluminium source (mol ratio) is also Na 3pO 412H 2o and step 1) in the mol ratio of Water Soluble Compound aluminium salt;
Crystal seed/aluminium source (mol ratio) is also sheet α-Al 2o 3the mol ratio of crystal seed and described Water Soluble Compound aluminium salt;
Table 2, embodiment 1-8 gained flake aluminum oxide feature
Embodiment Median size (μm) Mean thickness (μm) Radius-thickness ratio Reunite or twin
1 11 0.2 55 Nothing
2 12 0.2 60 Nothing
3 11 0.2 55 Nothing
4 15 0.3 50 Nothing
5 11 0.2 55 Nothing
6 14 0.3 47 Nothing
7 12 0.2 60 Nothing
8 13 0.2 65 Nothing

Claims (10)

1. prepare sheet α-Al for one kind 2o 3method, comprise the steps:
1) in the saturated aqueous solution of Water Soluble Compound aluminium salt, add crystal growth modifier, mixing obtains suspension liquid a;
2) in the aqueous solution of carbonate, Na is added 3pO 412H 2o, mixing obtains solution b;
3) when Keep agitation, by step 2) gained solution b joins step 1) in gained suspension liquid a, be hydrolyzed reaction, and react complete and dried by gained gel mixture, last calcining of pulverizing, obtains described sheet α-Al 2o 3.
2. method according to claim 1, is characterized in that: described step 1) in, Water Soluble Compound aluminium salt is selected from least one in 12 hydrazine aluminum sulfate potassium and sodium alum;
Described crystal growth modifier is water-soluble titanium salt;
Described water-soluble titanium salt is specifically selected from least one in titanyl sulfate and titanium tetrachloride;
The mol ratio of described crystal growth modifier and described Water Soluble Compound aluminium salt is 1:50-1:300;
Described step 2) in, carbonate is selected from least one in sodium carbonate and salt of wormwood;
Described carbonate and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 3:2;
Described Na 3pO 412H 2o and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 1:70-1:280;
Described step 3) in hydrolysis reaction step, temperature is room temperature, and the time is 0.5 hour-2 hours;
In described grinding steps, after grinding, the particle diameter of powder is 100 μm-200 μm;
In described calcining step, temperature is 1000 DEG C-1100 DEG C; Time is 3 hours-7 hours.
3. the sheet α-Al for preparing of the arbitrary described method of claim 1-3 2o 3.
4. sheet α-Al according to claim 3 2o 3, it is characterized in that: described sheet α-Al 2o 3mean thickness be 0.2 μm-0.5 μm;
Median size is 11 μm-13 μm;
Radius-thickness ratio >20.
5. prepare sheet α-Al for one kind 2o 3method, comprise the steps:
1) in the saturated aqueous solution of Water Soluble Compound aluminium salt, add crystal growth modifier and crystal seed, mixing obtains suspension liquid a;
Wherein, described crystal seed is the arbitrary described sheet α-Al of claim 3 or 4 2o 3;
2) in the aqueous solution of carbonate, Na is added 3pO 412H 2o, mixing obtains solution b;
3) when Keep agitation, by step 2) gained solution b joins step 1) in gained suspension liquid a, be hydrolyzed reaction, and react complete and dried by gained gel mixture, last calcining of pulverizing, obtains described sheet α-Al 2o 3.
6. method according to claim 5, is characterized in that: described step 1) in, Water Soluble Compound aluminium salt is selected from least one in 12 hydrazine aluminum sulfate potassium and sodium alum;
Described crystal growth modifier is water-soluble titanium salt;
Described water-soluble titanium salt is specifically selected from least one in titanyl sulfate and titanium tetrachloride;
The mol ratio of described crystal growth modifier and described Water Soluble Compound aluminium salt is 1:50-1:300;
Described sheet α-Al 2o 3the mol ratio of crystal seed and described Water Soluble Compound aluminium salt is 1:40-1:200;
Described step 2) in, carbonate is selected from least one in sodium carbonate and salt of wormwood;
Described carbonate and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 3:2;
Described Na 3pO 412H 2o and step 1) described in the mol ratio of Water Soluble Compound aluminium salt be 1:70-1:280;
Described step 3) in hydrolysis reaction step, temperature is room temperature, and the time is 0.5 hour-2 hours;
In described grinding steps, after grinding, the particle diameter of powder is 100 μm-200 μm;
In described calcining step, temperature is 850 DEG C-1100 DEG C; Time is 3 hours-7 hours.
7. the sheet α-Al for preparing of the arbitrary described method of claim 5 or 6 2o 3.
8. sheet α-Al according to claim 7 2o 3, it is characterized in that: described sheet α-Al 2o 3mean thickness be 0.2 μm-0.5 μm;
Median size is 11 μm-15 μm;
Radius-thickness ratio >20.
9. the arbitrary described sheet α-Al of claim 3 or 4 or 7 or 8 2o 3preparing the application in pearly pigment.
10. with the arbitrary described sheet α-Al of claim 3 or 4 or 7 or 8 2o 3for the pearly pigment of base material.
CN201510300413.6A 2015-06-03 2015-06-03 Method for preparing laminar alpha-Al2O3 pearlescent pigment base material by use of compound aluminum salt Pending CN104925843A (en)

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CN105731509A (en) * 2016-05-18 2016-07-06 湖北大学 Flaky alpha-Al2O3 powder and preparation method thereof
CN110407238A (en) * 2019-08-23 2019-11-05 济南大学 A kind of method that crystal seed method prepares flaky alpha-alumina crystals
CN111908502A (en) * 2020-06-25 2020-11-10 江阴市友佳珠光云母有限公司 Production process of colorful ultrathin synthetic mica sheet
KR102302448B1 (en) * 2021-01-12 2021-09-16 주식회사 티세라 Plate-shaped α-alumina particles and method thereof
CN114958035A (en) * 2022-06-06 2022-08-30 华南师范大学 Synthesis method of large-particle-size flaky alpha-alumina powder suitable for pearlescent pigment
CN115011142A (en) * 2022-07-19 2022-09-06 华南师范大学 Method for preparing alumina-based pearlescent pigment by hydrothermal method
CN116041984A (en) * 2022-12-30 2023-05-02 江苏贝丽得新材料有限公司 Flake alumina with self-weather-resistant function and preparation method thereof
CN115011142B (en) * 2022-07-19 2024-04-26 华南师范大学 Method for preparing aluminum oxide-based pearlescent pigment through hydrothermal method

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Publication number Priority date Publication date Assignee Title
CN105731509A (en) * 2016-05-18 2016-07-06 湖北大学 Flaky alpha-Al2O3 powder and preparation method thereof
CN110407238A (en) * 2019-08-23 2019-11-05 济南大学 A kind of method that crystal seed method prepares flaky alpha-alumina crystals
CN111908502A (en) * 2020-06-25 2020-11-10 江阴市友佳珠光云母有限公司 Production process of colorful ultrathin synthetic mica sheet
KR102302448B1 (en) * 2021-01-12 2021-09-16 주식회사 티세라 Plate-shaped α-alumina particles and method thereof
WO2022154227A1 (en) * 2021-01-12 2022-07-21 주식회사 티세라 Plate type α-alumina and manufacturing method therefor
CN114958035A (en) * 2022-06-06 2022-08-30 华南师范大学 Synthesis method of large-particle-size flaky alpha-alumina powder suitable for pearlescent pigment
CN115011142A (en) * 2022-07-19 2022-09-06 华南师范大学 Method for preparing alumina-based pearlescent pigment by hydrothermal method
CN115011142B (en) * 2022-07-19 2024-04-26 华南师范大学 Method for preparing aluminum oxide-based pearlescent pigment through hydrothermal method
CN116041984A (en) * 2022-12-30 2023-05-02 江苏贝丽得新材料有限公司 Flake alumina with self-weather-resistant function and preparation method thereof

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