CN101066841B - Process of preparing transparent glass ceramic with waste xiuyan jade - Google Patents

Process of preparing transparent glass ceramic with waste xiuyan jade Download PDF

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CN101066841B
CN101066841B CN2007100116385A CN200710011638A CN101066841B CN 101066841 B CN101066841 B CN 101066841B CN 2007100116385 A CN2007100116385 A CN 2007100116385A CN 200710011638 A CN200710011638 A CN 200710011638A CN 101066841 B CN101066841 B CN 101066841B
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waste
transparent glass
xiuyan jade
jade
glass ceramic
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CN101066841A (en
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张永明
李艳红
马晶
马雷
王慧华
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Abstract

The present invention relates to inorganic non-metallic material preparing technology, and is especially process of preparing transparent CaO-MgO-Al2O3-SiO2-F glass ceramic with waste Xiuyan jade. The material formulation has MgO content up to 20 wt% to lower the smelting point to 1350 deg.c, and fluoride, ZrO2 and TiO2 as crystal nucleus agent to obtain main crystal phase of fluorophlogopite andthe appearance effect similar to natural Xiuyan jade. The present invention makes it possible to make large scale artwork in low cost and has waste resource utilized reasonably to reduce environmental pollution.

Description

The method of preparing transparent glass ceramic with waste xiuyan jade
Technical field
The present invention relates to the preparation method of devitrified glass in a kind of ceramic, particularly relate to a kind of method with preparing transparent glass ceramic with waste xiuyan jade.
Background technology
Xiuyan jade (Xiuyanjade) is gained the name because of originating in Xiuyan county, China Liaoning Province, is one of Chinese four your name's jade.By the difference of mineralogical composition, the Xiuyan jade can be divided into three kinds of serpentine jade, tremolite jade, serpentine jade and tremolite jade mixtures, wherein based on the serpentine jade.Demonstrate the beautiful composition of serpentine according to the infrared absorption spectrum graphic representation, and contain a small amount of chrysotile, serpophite.The tremolite mainly is made up of the tremolite, and the chlorite jade mainly is made up of penninite.Also the beautiful segmentation in Xiuyan can be divided into beautiful three kinds of serpentine-jade, pattern jade, green mud by means such as microscope, transmission electron microscope, X-ray diffraction analysis, differential thermal analysis.
Aspect chemical ingredients, because the mineral compositions that different jade are planted in the jade of Xiuyan and the difference of symbiotic combination thereof, thereby its chemical ingredients also has bigger difference: the beautiful relative rich magnesium of serpentine, Silicon-rich, poor aluminium.The saturating relative Silicon-rich of the tremolite, rich calcium, poor magnesium, the then poor relatively magnesium of chlorite jade, poor silicon, rich aluminium.Serpentine is because the difference in symbiotic gangue ore deposit with it, thereby chemical ingredients is also different.Often near the theoretical content of the various components of serpentine minerals, symbiosis has the beautiful various components contents of the relatively poor serpentine of the quality of more gangue mineral then to change bigger to the chemical ingredients of the serpentine jade that general matter is pure.If be rich in silicate minerals, SiO then 2, CaO content increases, MgO content reduces.Following table is the chemical constitution of Xiuyan jade:
The chemical constitution table of Xiuyan jade
The Xiuyan jade is Chinese output maximum, most widely used a kind of jade always, is commonly used to produce jadeware.Produce a large amount of waste materials and environment structure is threatened in the course of processing, in view of the above, we are major-minor with other feedstock production CaO-MgO-Al according to its chemical constitution with waste xiuyan jade 2O 3-SiO 2-F system transparent glass ceramics.
Summary of the invention
The object of the present invention is to provide a kind of waste xiuyan jade that utilizes as main raw material, add other raw mineral materialss, industrial chemicals prepares transparent glass ceramics as auxiliary material, utilize discarded natural resources effective and reasonablely, reduce environmental pollution.By controlling nucleus agent and heat treating regime to obtain principal crystalline phase, make goods reach natural soapstone effect in appearance, can make imitative beautiful artwork.
The objective of the invention is to be achieved through the following technical solutions:
The method of preparing transparent glass ceramic with waste xiuyan jade, this method are main raw material, preparation CaO-MgO-Al with the waste xiuyan jade 2O 3-SiO 2-F system transparent glass ceramics, MgO quality percentage composition is 5~20% in the prescription, F quality percentage composition is 4~7%.
The method of described preparing transparent glass ceramic with waste xiuyan jade, MgO is introduced by waste xiuyan jade in its prescription, and F is by AlF 3, Na 2SiF 6, Na 3AlF 6The form of wherein one or more is introduced.
The method of described preparing transparent glass ceramic with waste xiuyan jade, its method obtains trichroite, fluorophlogopite principal crystalline phase through Overheating Treatment.
The method of described preparing transparent glass ceramic with waste xiuyan jade, the temperature of fusion of this method parent glass are 1150~1350 ℃, and crystallization temperature is 600~950 ℃.
The method of described preparing transparent glass ceramic with waste xiuyan jade, this method adopt transition metal oxide or rare earth oxide as tinting material they into shades of colour.
Advantage of the present invention and effect are:
Utilize waste xiuyan jade as main raw material, add other raw mineral materialss, industrial chemicals prepares transparent glass ceramics as auxiliary material, control nucleus agent and heat treating regime are to obtain principal crystalline phase, its goods reach natural soapstone effect in appearance, because technology is simple, cost is low and can make the artwork of big specification, therefore have extremely vast market prospect, can utilize discarded natural resources simultaneously effective and reasonablely, reduce environmental pollution.
Description of drawings
Accompanying drawing is preparation technology's flow diagram of transparent glass ceramics of the present invention.
Embodiment
The present invention is described in detail with reference to the accompanying drawings.
1, raw material: waste xiuyan jade, Wingdale, silica, fluorite, sodium aluminum fluoride, AlF 3, Na 2SiF 6, ZrO 2, TiO 2
2, technical formula: SiO 256~60%, Al 2O 312~20%, MgO5~20%, CaO5~10%, F4~7%.
3, operational path: the granularity that above-mentioned raw mineral materials is processed into requirement, mix after the accurate weighing by prescription with industrial chemicals, the high alumina crucible of packing into, put in the globars electric furnace and be heated to design temperature, be incubated 1 hour, put into retort furnace after pouring into the cast iron die for molding, setting insulation annealing in 2 hours under the temperature.Sample after the annealing is loaded program in the pilot circuit, under the system of setting, heat-treat, carry out cold working behind the cool to room temperature and obtain desired goods.
Embodiment 1
With waste xiuyan jade, it is 250 order all-pass mistakes that Wingdale, silica, fluorite, sodium aluminum fluoride are processed into granularity.Calculate the consumption of above-mentioned raw materials by the chemical ingredients of table 1, with ZrO 2, TiO 2In ball mill, mix together, in the corundum crucible of packing into, send into and be heated to 1290 ℃ in the globars electric furnace, be incubated 1 hour, take out and pour into the cast iron die for molding, in 500 ℃ of retort furnaces, anneal.Send into again in the retort furnace after the sample cooling, after 2 hours, rise to 690 ℃ of insulations 30 minutes, naturally cool to room temperature after turning off power supply with 20 ℃/minute temperature rise rates 650 ℃ of insulations.This sample polishing, polishing back obtain finished product.
Embodiment 2
With waste xiuyan jade, it is 250 order all-pass mistakes that Wingdale, silica, fluorite, sodium aluminum fluoride are processed into granularity.Calculate the consumption of above-mentioned raw materials by the chemical ingredients of table 2, with ZrO 2, TiO 2In ball mill, mix together, in the corundum crucible of packing into, send into and be heated to 1210 ℃ in the globars electric furnace, be incubated 1 hour, take out and pour into the cast iron die for molding, in 500 ℃ of retort furnaces, anneal.Send into again in the retort furnace after the sample cooling, after 2 hours, rise to 680 ℃ of insulations 30 minutes, naturally cool to room temperature after turning off power supply with 20 ℃/minute temperature rise rates 630 ℃ of insulations.This sample polishing, polishing back obtain finished product.
Embodiment 3
With waste xiuyan jade, it is 250 order all-pass mistakes that Wingdale, silica, fluorite are processed into granularity.Calculate the consumption of above-mentioned raw materials by the chemical ingredients of table 3, with AlF 3, ZrO 2, TiO 2In ball mill, mix together, in the corundum crucible of packing into, send into and be heated to 1350 ℃ in the globars electric furnace, be incubated 1 hour, take out and pour into the cast iron die for molding, in 500 ℃ of retort furnaces, anneal.Send into again in the retort furnace after the sample cooling, after 2 hours, rise to 730 ℃ of insulations 30 minutes, naturally cool to room temperature after turning off power supply with 20 ℃/minute temperature rise rates 680 ℃ of insulations.This sample polishing, polishing back obtain finished product.
Embodiment 4
With waste xiuyan jade, it is 250 order all-pass mistakes that Wingdale, silica, fluorite are processed into granularity.Calculate the consumption of above-mentioned raw materials by the chemical ingredients of table 3, with Na 2SiF 6, ZrO 2, TiO 2In ball mill, mix together, in the corundum crucible of packing into, send into and be heated to 1150 ℃ in the globars electric furnace, be incubated 1 hour, take out and pour into the cast iron die for molding, in 500 ℃ of retort furnaces, anneal.Send into again in the retort furnace after the sample cooling, after 2 hours, rise to 650 ℃ of insulations 30 minutes, naturally cool to room temperature after turning off power supply with 20 ℃/minute temperature rise rates 600 ℃ of insulations.This sample polishing, polishing back obtain finished product.
Following table 1 to table 4 is the quality percentage composition of the various compositions in the component design and the quality percentage composition in the actual glass pottery.
Table 1
Figure S07111638520070711D000051
Table 2
Figure S07111638520070711D000061
Table 3
Figure S07111638520070711D000062
Table 4
Figure S07111638520070711D000071

Claims (6)

1. the method for preparing transparent glass ceramic with waste xiuyan jade is characterized in that this method is main raw material, preparation CaO-MgO-Al with the waste xiuyan jade 2O 3-SiO 2-F system transparent glass ceramics, SiO in the prescription 256~60%, Al 2O 312~20%, MgO 5~20%, and CaO 5~10%, and F 4~7%; The temperature of fusion of this method parent glass is 1150~1350 ℃, and crystallization temperature is 600~950 ℃.
2. the method for preparing transparent glass ceramic with waste xiuyan jade according to claim 1 is characterized in that MgO is introduced by waste xiuyan jade in the prescription, and F is by AlF 3, Na 2SiF 6, Na 3AlF 6A kind of form is wherein introduced.
3. the method for preparing transparent glass ceramic with waste xiuyan jade according to claim 1 is characterized in that MgO is introduced by waste xiuyan jade in the prescription, and F is by AlF 3, Na 2SiF 6, Na 3AlF 6The form of wherein more than one is introduced.
4. the method for preparing transparent glass ceramic with waste xiuyan jade according to claim 1 is characterized in that this method obtains trichroite, fluorophlogopite principal crystalline phase through Overheating Treatment.
5. the method for preparing transparent glass ceramic with waste xiuyan jade according to claim 1 is characterized in that this method adopts transition metal oxide as tinting material it into shades of colour.
6. the method for preparing transparent glass ceramic with waste xiuyan jade according to claim 5 is characterized in that, described transition metal oxide is a rare earth oxide.
CN2007100116385A 2007-06-08 2007-06-08 Process of preparing transparent glass ceramic with waste xiuyan jade Expired - Fee Related CN101066841B (en)

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Publication number Priority date Publication date Assignee Title
CN102617115B (en) * 2011-01-28 2015-01-07 北京宝泰云母新材料科技有限公司 Composition and method for smelting fluorophlogopite ceramic, and fluorophlogopite ceramic prepared from composition
CN102417305B (en) * 2011-06-14 2013-12-11 淄博工陶耐火材料有限公司 Artificial jade dishware and preparation method thereof
CN103408286B (en) * 2013-06-24 2016-05-11 徐传德 A kind of preparation method of large-scale jade construction material
CN103508728A (en) * 2013-06-24 2014-01-15 徐传德 Preparation method of jade article tableware
RU2574642C1 (en) * 2014-12-29 2016-02-10 Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" Method for obtaining fused-cast potassium fluorophlogopite

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB986289A (en) * 1962-10-30 1965-03-17 British Iron Steel Research A material produced by devitrification of a glass made from a metallurgical slag
SU1237645A1 (en) * 1985-01-04 1986-06-15 Белорусский Ордена Трудового Красного Знамени Технологический Институт Им.С.М.Кирова Glass for glass-crystal material
CN85108548A (en) * 1985-04-15 1986-10-15 康宁玻璃厂 The enhancing of alkaline earth aluminosilicate glass-ceramics
CN1762878A (en) * 2004-10-18 2006-04-26 成都理工大学 Artificial diopside material and its preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB986289A (en) * 1962-10-30 1965-03-17 British Iron Steel Research A material produced by devitrification of a glass made from a metallurgical slag
SU1237645A1 (en) * 1985-01-04 1986-06-15 Белорусский Ордена Трудового Красного Знамени Технологический Институт Им.С.М.Кирова Glass for glass-crystal material
CN85108548A (en) * 1985-04-15 1986-10-15 康宁玻璃厂 The enhancing of alkaline earth aluminosilicate glass-ceramics
CN1762878A (en) * 2004-10-18 2006-04-26 成都理工大学 Artificial diopside material and its preparation method

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