TWI465526B - A means for the synthesis of ultramarine from mica powder - Google Patents
A means for the synthesis of ultramarine from mica powder Download PDFInfo
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- TWI465526B TWI465526B TW102111821A TW102111821A TWI465526B TW I465526 B TWI465526 B TW I465526B TW 102111821 A TW102111821 A TW 102111821A TW 102111821 A TW102111821 A TW 102111821A TW I465526 B TWI465526 B TW I465526B
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- ultramarine
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Description
本創作屬於以天然礦物資源合成高經濟價值產物之技術領域。This creation belongs to the technical field of synthesizing high economic value products with natural mineral resources.
群青(ultramarine)是一種性質穩定,耐風化、耐鹼、耐高溫,以青金石為主要組成之礦物顏料。青金石之化學式為Na8 Al6 Si6 O24 (S2 ,S3 ),為等軸晶系之礦物,結晶呈菱形十二面體,具有{011}不完全解理面,斷口呈參差不齊,莫式硬度為5~5.5,比重2.4-2.45,玻璃光澤,半透明,藍綠色,在火焰試驗中會發出強烈的黃光,為Na+ 發出之光譜。青金石之結晶結構為一個以Si4+ 、Al3+ 、Na+ 等陽離子組成之方鈉石β籠,內含有Sx - (x=2-4)陰離子團,以維持電荷平衡,並且為藍色及黃色之發色體(chromophore)。工業用群青均以人工方式合成,品質較天然者純。Ultramarine is a mineral pigment with stable properties, weathering resistance, alkali resistance and high temperature resistance, with lapis lazuli as the main component. The chemical formula of lapis lazuli is Na 8 Al 6 Si 6 O 24 (S 2 , S 3 ), which is a mineral of equiaxed crystal system. The crystal is rhombohedral dodecahedron with {011} incomplete cleavage plane, and the fracture is staggered. Mismatched, Mo type hardness is 5~5.5, specific gravity is 2.4-2.45, glass luster, translucent, blue-green, strong yellow light will be emitted in the flame test, which is the spectrum emitted by Na + . The crystal structure of lapis lazuli is a sodalite β cage composed of cations such as Si 4+ , Al 3+ , Na + , etc., containing S x - (x=2-4) anion groups to maintain charge balance, and Blue and yellow chromophore. Industrial greens are synthesized by artificial means, and the quality is purer than natural ones.
國內外合成群青使用之原料有高嶺土、禾樂石、天然沸石、飛灰、含矽/鋁/鈉之氧化物等,並未有以本發明所使用之雲母粉(含絹雲母及葉蠟石)為原料。The raw materials used for synthesizing ultramarine at home and abroad include kaolin, Helestone, natural zeolite, fly ash, cerium/aluminum/sodium oxide, etc., and there is no mica powder (including sericite and pyrophyllite) used in the present invention. ) as raw materials.
本發明為將雲母粉研磨,與碳酸鈉(Na2 CO3 )、硫(S)、活性碳(C)混合,在大氣氣氛下,先於700℃至1000℃之溫度,再於300℃至500℃之溫度,分別煆燒1至16小時,即可合成群青,內容主要如下:將雲母粉研磨至10 μm以下(中位粒徑d50 0.6 μm,比表面積50 m2 /g),與碳酸鈉(Na2 CO3 )、硫(S)、活性碳(C)混合,四種原料質量比為1:(0.33~3):(0.5~2):(0.05~0.5),將此混合物在大氣氣氛下,加熱至700℃至1000℃之溫度範圍,並在該溫度維持1小時至16小時,隨後降溫至300℃至500℃之溫度範圍,並在該溫度維持1小時至16小時,反應完成後,將固體產物水洗及過濾,固體部份再加工研磨,即為群青。The invention is characterized in that the mica powder is ground and mixed with sodium carbonate (Na 2 CO 3 ), sulfur (S) and activated carbon (C), in an air atmosphere, before the temperature of 700 ° C to 1000 ° C, and then at 300 ° C. The temperature of 500 ° C, respectively, calcined for 1 to 16 hours, you can synthesize ultramarine, the main content is as follows: grinding mica powder below 10 μm (median diameter d 50 0.6 μm, specific surface area 50 m 2 /g), mixed with sodium carbonate (Na 2 CO 3 ), sulfur (S), activated carbon (C), the mass ratio of the four raw materials is 1: (0.33~3): (0.5~2): ( 0.05~0.5), the mixture is heated to a temperature range of 700 ° C to 1000 ° C under an air atmosphere, and maintained at this temperature for 1 hour to 16 hours, and then cooled to a temperature range of 300 ° C to 500 ° C, and The temperature is maintained for 1 hour to 16 hours. After the reaction is completed, the solid product is washed with water and filtered, and the solid portion is further processed and ground to obtain ultramarine blue.
第一圖本發明「雲母合成群青之方法」之流程圖。The first figure is a flow chart of the "method of synthesizing ultramarine in mica" of the present invention.
附件一本發明使用原料之X光繞射圖型。Annex I The invention uses an X-ray diffraction pattern of the raw material.
附件二經本發明之方法,產物之X光繞射圖型。Annex II X-ray diffraction pattern of the product by the method of the invention.
附件三經本發明之方法,產物之拉曼(Raman)吸收光譜。Annex III Raman absorption spectra of the product by the method of the invention.
附件四經本發明之方法,雲母研磨樣為起始原料,Na2 CO3 /S比及煅燒溫度二因子影響下之產物顏色。Annex IV According to the method of the present invention, the mica grinding sample is the starting material, the color of the product under the influence of the Na 2 CO 3 /S ratio and the calcination temperature.
附件五經本發明之方法,Na2 CO3 /S比及煅燒溫度二因子影響下之霞石、青金石結晶區域圖。Annex V is a graph of the crystalline region of nepheline and lapis lazuli under the influence of the Na 2 CO 3 /S ratio and the calcination temperature by the method of the present invention.
附件六經本發明之方法,產物之電子顯微鏡照片。Annex VI Electron micrograph of the product by the method of the invention.
本發明之實施方法示於第一圖,將雲母粉研磨至10 μm以下(中位粒徑d50 0.6 μm,比表面積50 m2 /g),此-10 μm之固體「11」,與碳酸鈉(Na2 CO3 )「12」、硫(S)「13」、活性碳(C)「14」混合「2」,四種原料質量比為1:(0.33~3):(0.5~2):(0.05~0.5),將此混合物在大氣氣氛下,加熱至700℃至1000℃之溫度範圍,並在該溫度維持1小時至16小時,隨後降溫至300℃至500℃之溫度範圍,並在該溫度維持1小時至16小時「3」,反應完成後,廢氣「32」回收處理,固體產物「31」水洗及過濾「4」,濾液「42」回收處理,固體「41」烘乾「5」,研磨「6」即為群青「61」。The method for carrying out the invention is shown in the first figure, and the mica powder is ground to below 10 μm (median particle diameter d 50 0.6 μm, specific surface area 50 m 2 /g), this -10 μm solid "11", mixed with sodium carbonate (Na 2 CO 3 ) "12", sulfur (S) "13", activated carbon (C) "14""2" The mass ratio of the four raw materials is 1: (0.33~3): (0.5~2): (0.05~0.5), and the mixture is heated to a temperature range of 700 ° C to 1000 ° C under an atmospheric atmosphere, and at the temperature Maintaining for 1 hour to 16 hours, then cooling to a temperature range of 300 ° C to 500 ° C, and maintaining the temperature for 1 hour to 16 hours "3". After the reaction is completed, the exhaust gas "32" is recovered and the solid product "31" is washed. And filter "4", the filtrate "42" is recycled, the solid "41" is dried "5", and the polishing "6" is the ultramarine "61".
11‧‧‧雲母粉(-10 μm)11‧‧‧mica powder (-10 μm)
12‧‧‧碳酸鈉(Na2 CO3 )12‧‧‧Sodium carbonate (Na 2 CO 3 )
16‧‧‧硫(S)16‧‧‧Sulphur (S)
14‧‧‧活性碳(C)14‧‧‧Active carbon (C)
2‧‧‧固體原料之混合2‧‧‧Mixed solid materials
21‧‧‧反應原料21‧‧‧Reactive raw materials
3‧‧‧反應3‧‧‧Reaction
31‧‧‧反應產物31‧‧‧Reaction products
4‧‧‧水洗過濾4‧‧‧Washing filtration
41‧‧‧濾液41‧‧‧ filtrate
42‧‧‧固體42‧‧‧ Solid
5‧‧‧烘乾5‧‧‧Drying
6‧‧‧研磨6‧‧‧ grinding
61‧‧‧群青61‧‧‧Qingqing
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113072822A (en) * | 2021-04-07 | 2021-07-06 | 南京工业大学 | Preparation method of blue pearlescent pigment based on ultramarine pigment |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1239080A (en) * | 1917-01-11 | 1917-09-04 | Laurenz Bock | Manufacture of ultramarine. |
US2700618A (en) * | 1952-04-22 | 1955-01-25 | American Cyanamid Co | Manufacture of ultramarine |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1239080A (en) * | 1917-01-11 | 1917-09-04 | Laurenz Bock | Manufacture of ultramarine. |
US2700618A (en) * | 1952-04-22 | 1955-01-25 | American Cyanamid Co | Manufacture of ultramarine |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113072822A (en) * | 2021-04-07 | 2021-07-06 | 南京工业大学 | Preparation method of blue pearlescent pigment based on ultramarine pigment |
CN113072822B (en) * | 2021-04-07 | 2021-12-28 | 南京工业大学 | Preparation method of blue pearlescent pigment based on ultramarine pigment |
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