CN1609028A - Technology of sintering waste glass for preparing fluoro mica glass ceramic - Google Patents
Technology of sintering waste glass for preparing fluoro mica glass ceramic Download PDFInfo
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- CN1609028A CN1609028A CN 200310104932 CN200310104932A CN1609028A CN 1609028 A CN1609028 A CN 1609028A CN 200310104932 CN200310104932 CN 200310104932 CN 200310104932 A CN200310104932 A CN 200310104932A CN 1609028 A CN1609028 A CN 1609028A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract
The technological process of sintering waste glass for preparing fluoro mica glass ceramic includes the steps of selecting waste glass, washing and crushing to obtain glass powder; and features that into glass powder, 15-75 wt% fluoro mica crystal powder is added, and PVC adhesive in 2-10 wt% of the mixture is then added before molding and sintering in common electric furnace at normal pressure to produce fluoro mica glass ceramic. Compared with available glass ceramic producing process, the present invention has low production cost, simple production process, no need of melting glass and sintering separation, low sintering temperature, low power consumption and other advantages. Utilizing the technology of the present invention can producing while glass ceramic with pressure strength of 200-300 MPa, density 2.0-2.6 g/cu cm, and excellent machining performance of being drilling hole and turning with common cutter.
Description
[technical field] the present invention relates to a kind ofly utilize cullet sintering preparation can process fluorine mica glass-ceramic technology, particularly be raw material, add the fluorine mica powder, after the compression molding with the cullet, prepare the production technology of workable glass ceramic by sintering process, belong to engineering ceramic material and make the field.
[background technology] workable glass ceramic is a kind of matrix material of being made up of fluorine mica crystal and glass, and last century, the seventies at first came out in the U.S..It promptly has advantages such as stupalith electrical isolation, high temperature resistant, anti-oxidant, resistance to chemical attack, anti-thermal shock, overcome the unmanageable shortcoming of stupalith again, can use universal cutter by car, mill, dig, bore and be machined to precise measure, be the novel hi-tech fine ceramics material that a kind of utmost point has development potentiality, purposes is widely arranged in industrial production.Only have the U.S., Japan to produce in batches in the world at present, also there is produced in small quantities in China.Production technique is mainly scorification, and technical process is: batching → fusing → cast molding → two step thermal treatment crystallizatioies.The reputable brand Macor workable glass ceramic of Corning Incorporated just is to use this explained hereafter.Its raw material consists of: SiO
2-MgO-Al
2O
3-K
2O-B
2O
3-F 1500 ℃ of fusings, after the cast molding cooling, 800 ℃ of-1100 ℃ of thermal treatments, separates out fluorophlogopite respectively from glass.Developed sintering process in recent years again, technical process is: batching → fusing → shrend → pulverizing → compression molding → sintering crystallization.As U.S. Pat 5061308 (Method of manufacturingreadily machinable high strength glass ceramics) report, 1 (11～11.5%K will prepare burden
2O, 23.5～24.8%Mgo, 55～56.8%SiO
2, 8.4～12.6%F, 0.86～0.99%ZrO
2) and batching 2 (5～46%K
2O, 9.5～11%MgO, 46～48%SiO
2, 21～23%CaO, 0.2～0.5%CaF
2, 5～6.5%MgF, 8～8.5%P
2O
5) 1400 ℃～1500 ℃ fusings respectively, after the cooling, grind into powder mixes 30～95% powder 1 and 5～70% powder 2 again, compression molding under 200MPa pressure, and the mold pressing blank is made workable glass ceramic at 1050 ℃～1150 ℃ following sintering.There is following shortcoming in these two kinds of technologies: 1, glass melting temperature height (＞1500 ℃), and energy consumption is big; 2, the step thermal treatment of two in scorification crystallization process complexity; 3, in order in glass, to separate out the fluorophlogopite crystal, component of glass raw material there is strict restriction, can't uses common frit, must use industrial chemicals.All these causes the workable glass ceramic cost high, and the existing market price is 300～400 yuan/kg.Although thereby this material still is difficult to apply aborning to come out for many years so far.
According to the statistics made by the departments concerned, the annual cullet that produces of China has made full use of this considerable renewable resource up to 1,040 ten thousand tons, will play immeasurable effect to the Economic development of China.The recycling of cullet at present mainly contains: glass melts down and produces material of construction, as utilizes cullet to make glass Mosaic, artificial marble, granolith, floor tile, building decorative plate etc.The existing many patent reports of this respect are as Chinese patent notification number CN1016312, notification number CN1018526, notification number CN1062714, notification number CN1172089.There is report to say that Finland English Nola west company has invented recently and utilizes cullet to produce the patented technology of New Building Materials " ecological glass veneer ", dropped into and put into serial production.But the technology of utilizing cullet to produce workable glass ceramic at home and abroad is not reported, utilize cullet to produce the production cost that workable glass ceramic promptly can reduce workable glass ceramic, for the recycling of cullet opens up a new way, has the effect of double gain again.
[summary of the invention] the objective of the invention is the drawback at existing workable glass ceramic production method, on technology and on the raw material, it is improved, its innovation part is to adopt with after fluorine mica crystal powder and the direct mixing of cullet powder, under normal pressure, be sintered directly into workable glass ceramic, simplified production technique greatly, reduced production cost, both, also opened up a new way for the recycling of cullet for the condition created of applying of this hi-tech material.
The objective of the invention is to realize by following technique means.
A kind ofly utilize cullet sintering preparation can process fluorine mica glass-ceramic technology, comprise steps A with the cullet sorting, clean, pulverize and produce brokenly the glass powder, characteristics of the present invention are that step B mixes an amount of fluorine mica crystal powder by weight percentage in glass powder; Step C adds the suitable amount of adhesive compression molding in glass powder and fluorine mica crystal powder powder mix; Step D, makes and can process the fluorine mica glass-ceramic above-mentioned glass powder and fluorine mica crystal powder and binder blend sintering in the normal pressure atmosphere with process furnace.
Described steps A with colourless sheet glass, window glass and coloured container glass, window glass separately, is removed metal and the nonmetal foreign material that wait at first cullet being carried out sorting, cleans up back classification ball milling and makes glass powder below 100 orders.Because different sorts glass has different performances, made added glass-ceramic performance is also different.Described step B mixes 15～75% fluorine mica crystal powder by weight percentage in the cullet powder, even with thorough mixing in the stirrer.Described step C adds that to account for glass powder and fluorine mica crystal powder powder mix weight ratio be 2～10% binding agent in glass powder and fluorine mica crystal powder powder mix.With above-mentioned glass powder and fluorine mica crystal powder and binder blend extrusion forming, pressure is 50～350MPa in mould.The workpiece that size is big also needs further isostatic cool pressing under 100～200MPa, so that biscuit density is more even.Described step D be with molding biscuit in process furnace such as common electric furnace, electric heating roller kiln, under 500 ℃～700 ℃ temperature, be incubated 1～10 hour, binding agent is removed in oven dry; Temperature is warming up to 800 ℃～1200 ℃, sintering time determines that according to workpiece size general soaking time is 1～10 hour, cools to room temperature with the furnace and comes out of the stove again, and sintering is made and can be processed fluorine mica glass-ceramic finished product.
Above-mentioned fluorine mica can select for use fluorophlogopite, fluorine calcium mica, fluorine roscoelite, fluorine boron mica, fluorine silicon mica any one, or select for use fluorophlogopite, fluorine calcium mica, fluorine roscoelite, fluorine boron mica, two or more component arbitrary combination of fluorine silicon mica to mix fluorine mica.
Above-mentioned tackiness agent is the PVC tackiness agent.
The production technology of utilizing cullet to prepare workable glass ceramic provided by the present invention, the main technique flow process is: cullet sorting, cleaning; Ball mill pulverizing; Mix fluorine mica and tackiness agent compression molding; Sintering.This method is to existing workable glass ceramic production method---and scorification has carried out reform completely, directly adopts cullet on raw material, turns waste into wealth; On technology, adopt sintering process, needn't molten glass, save energy, production technique is simple, is domestic and international initiative.Be workable glass ceramic a kind of new production technique is provided, opened up a new way for the recycling of cullet again, greatly reduce the production cost of workable glass ceramic, remarkable economic efficiency and social benefit are arranged.Prepared workable glass ceramic uses that common machining apparatus and cutter can be holed, tapping, turning, has good processability, is a kind of novel hi-tech fine ceramics material, and purposes is widely arranged in industrial production.
The present invention and existing workable glass ceramic production technology relatively, it is low to have a production cost, production technique is simple, need not molten glass, also need not the sintering crystallization, sintering temperature is low, advantages such as save energy.The workable glass ceramic color of utilizing present technique to produce is pure white, ultimate compression strength 200～300MPa, density 2.0～2.6g/cm
3, having good processability, available universal cutter is holed and turning on common machining equipment.
The workable glass ceramic that utilizes the technology of the present invention to produce is a kind of good high temperature resistant electrically insulating material, and it has very high electric simulation strength, high volume resistance and low dielectric loss.Simultaneously be again a kind of can be in the very low temperature field widely used anti-corrosion electric insulating material.Its use range can be used in many electrical equipments at-270 ℃～+ 800 ℃.Because the mica crystal in the workable glass ceramic has certain elasticity, can prevent the expansion of tiny crack, so it has thermal shock resistance preferably again, from 800 ℃ be chilled to 0 ℃ not broken, 200 ℃ are quenched to 0 ℃ of intensity and do not change.Its low thermal coefficient of expansion has guaranteed the dimensional stabilizing of workpiece, can carry out airtight sealed knot.Because workable glass ceramic has various excellent comprehensive performances, can satisfy the high precision technology requirement, need not die design and making, shorten the lead time greatly, can quicken engineering progress, save development cost, therefore be subjected to the welcome of vast scientific research, teaching and design department deeply, in industrial production fields such as Aeronautics and Astronautics, electronic substrates, high-temperature insulation skeleton, ion film plating, vacuum plating, ion microscope, ion accelerator, laser apparatus, medical facilities, precision meter, cryogenic engineering, purposes widely arranged.The workable glass ceramic that adopts present technique to produce is low owing to cost, and technology is simple, will further enlarge the application of this material in industrial circle.
Implement the technology of the present invention and do not need specific installation, only need common industrial ceramics production unit: as pulverizer, ball mill, pressing machine, sintering oven, engine lathe, drilling machine etc. just can be produced qualified product, has low equipment investment, production process is pollution-free, characteristics such as added value of product height are new technologies that is worth promoting.
[embodiment]
Embodiment one: at first cullet is carried out sorting, after colourless sheet glass was cleaned up, ball milling was made 200 order glass powder.Mix 50% fluorophlogopite crystal powder by weight percentage at above-mentioned cullet powder, even with thorough mixing in the stirrer.Add that to account for glass powder and fluorophlogopite crystal powder powder mix weight ratio be 8% PVC binding agent.With above-mentioned glass powder and fluorine mica crystal powder and binder blend extrusion forming, pressure is 300MPa in mould, so that biscuit density is more even.It is 500 ℃～700 ℃ common electric furnaces that molding biscuit is put into temperature, is incubated oven dry in 5～7 hours, removes binding agent; Temperature is warming up to 800 ℃～1200 ℃ again, is incubated 6～8 hours, cool to room temperature with the furnace and come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
Embodiment two: at first cullet is carried out sorting, with colourless sheet glass, window glass and coloured container glass, window glass separately, clean up back classification ball milling and make the following glass powder of 100 orders.In the cullet powder, mix 35% fluorine calcium mica crystal powder by weight percentage, even with thorough mixing in the stirrer.Adding that to account for glass powder and fluorine calcium mica crystal powder powder mix weight ratio be 5% PVC binding agent, is extrusion forming in the 350MPa mould at pressure.Molding biscuit is incubated 8 hours down at 600 ℃ in common electric furnace, binding agent is removed in oven dry, is warming up to 1000 ℃ of insulations 10 hours again, cools to room temperature with the furnace to come out of the stove, and sintering is made and can be processed fluorine mica glass-ceramic finished product.
Embodiment three: ball milling was made the glass powder below 150 orders after window glass was cleaned up, and added 60% fluorine roscoelite crystal powder in the cullet powder by weight percentage, and is even with the stirrer thorough mixing.Add again that to account for glass powder and fluorine roscoelite crystal powder powder mix weight ratio be 3% PVC binding agent, extrusion forming in mould, pressure is 100～350MPa.With the oven dry in 5 hours of insulation during molding biscuit is in 600 ℃ of common electric furnaces, removal binding agent, be warming up to 800 ℃ again, be incubated 5 hours, cool to room temperature with the furnace and come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
Embodiment four: after coloured container glass is cleaned up, ball milling is made the following glass powder of 100 orders, in the cullet powder, add 30% any two kinds of random blended fluorine of ratio boron micas, fluorine silicon mica crystal powder by weight percentage, even with thorough mixing in the stirrer.Add that to account for glass powder and fluorine boron mica, fluorine silicon mica crystal powder powder mix weight ratio be 7% PVC binding agent, at pressure is extrusion forming in the mould of 350MPa, the big workpiece of size also needed under 100～200MPa further isostatic cool pressing 1～3 hour, so that biscuit density is more even.Molding biscuit is incubated oven dry in 4～7 hours down at 550 ℃～650 ℃, removes binding agent in the electric heating roller kiln, be warming up to 850 ℃～1100 ℃ again, sintering time determines according to workpiece size, general insulation 5～6 hours, cool to room temperature with the furnace and come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
Embodiment five: after coloured container glass is cleaned up, ball milling is made the following glass powder of 150 orders, in the cullet powder, add 25% fluorophlogopite, fluorine calcium mica, fluorine roscoelite, fluorine boron mica, two or more component arbitrary combination blended fluorine mica crystal powder of fluorine silicon mica by weight percentage, even with thorough mixing in the stirrer.Add that to account for glass powder and fluorine mica crystal powder powder mix weight ratio be 9% PVC binding agent, at pressure is extrusion forming in the mould of 250MPa, the big workpiece of size also needed under 150～190MPa further isostatic cool pressing 1～3 hour, so that biscuit density is more even.Molding biscuit is incubated oven dry in 4～7 hours down at 550 ℃～650 ℃, removes binding agent in the electric heating roller kiln, be warming up to 850 ℃～1100 ℃ again, be incubated 5～6 hours, cool to room temperature with the furnace to come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
Claims (9)
1, a kind ofly utilize cullet sintering preparation can process fluorine mica glass-ceramic technology, comprise steps A with the cullet sorting, clean, pulverize and produce glass powder, characteristics of the present invention are that step B mixes an amount of fluorine mica crystal powder by weight percentage in glass powder; Step C adds the suitable amount of adhesive compression molding in glass powder and fluorine mica crystal powder powder mix; Step D, makes and can process the fluorine mica glass-ceramic above-mentioned glass powder and fluorine mica crystal powder and binder blend sintering in the normal pressure atmosphere with process furnace.
2, preparation workable glass ceramic technology according to claim 1 is characterized in that said step B mixes 15～75% fluorine mica crystal powder by weight percentage in the cullet powder, and is even with thorough mixing in the stirrer.
3, preparation workable glass ceramic technology according to claim 1 and 2, it is characterized in that said fluorine mica can select for use fluorophlogopite, fluorine calcium mica, fluorine roscoelite, fluorine boron mica, fluorine silicon mica any one, or select fluorophlogopite, fluorine calcium mica, fluorine roscoelite, fluorine boron mica, two or more component arbitrary combination fluorine mica of fluorine silicon mica for use.
4, preparation workable glass ceramic technology according to claim 1 and 2, it is characterized in that said step C is in glass powder and fluorine mica crystal powder powder mix, add that to account for glass powder and fluorine mica crystal powder powder mix weight ratio be 2～10% binding agent, mix following extrusion forming at 50～350MPa.
5, preparation workable glass ceramic technology according to claim 4 is characterized in that the extrusion forming workpiece also needs further isostatic cool pressing under 100～200MPa.
6, according to claim 1,2 or 5 described preparation workable glass ceramic technology, it is characterized in that said step D is the mold pressing biscuit, in process furnace, be incubated oven dry in 1～10 hour down, remove binding agent at 500 ℃～700 ℃, be warming up to 800 ℃～1200 ℃ again, be incubated 1～10 hour, cool to room temperature with the furnace and come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
7, preparation workable glass ceramic technology according to claim 4, it is characterized in that said D step is the mold pressing biscuit, in process furnace such as common electric furnace, be incubated oven dry in 1～10 hour down, remove binding agent at 500 ℃～700 ℃, be warming up to 800 ℃～1200 ℃ again, be incubated 1～10 hour, cool to room temperature with the furnace and come out of the stove, sintering is made and can be processed fluorine mica glass-ceramic finished product.
8, preparation workable glass ceramic technology according to claim 1, it is characterized in that said steps A is to divide clear plate glass and window glass with cullet, coloured container glass and coloured window glass, remove metal and foreign material such as nonmetal, flush away dirt and oil stain dry the back classification and send into the glass powder that is crushed in the ball mill below 100 orders.
9, preparation workable glass ceramic technology according to claim 1 and 2 is characterized in that said tackiness agent is the PVC tackiness agent.
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| CN1915878B (en) * | 2006-09-05 | 2010-09-01 | 山东建筑大学材料科学研究所 | Method for producing color glass ceramic by using sludge of concrete |
| CN101844869A (en) * | 2010-05-24 | 2010-09-29 | 大连交通大学 | Method for preparing fluorine amphibole glass ceramic by using reactive crystallization-sintering method |
| CN102344251A (en) * | 2011-07-20 | 2012-02-08 | 大连交通大学 | Preparation method for lepidolite glass ceramic |
| CN102617115A (en) * | 2011-01-28 | 2012-08-01 | 吕宝林 | Composition and method for smelting fluorophlogopite ceramic, and fluorophlogopite ceramic prepared from composition |
| CN104250067A (en) * | 2013-06-28 | 2014-12-31 | 中国地质大学（北京） | Method for preparation of machinable mica glass ceramic insulating material from waste glass and phlogopite |
| CN104973787A (en) * | 2015-06-10 | 2015-10-14 | 安徽省德邦瓷业有限公司 | Ageing-resistant glass ceramic disc and preparation method thereof |
| CN105906212A (en) * | 2016-04-21 | 2016-08-31 | 中南大学 | Mica-based glass ceramic and preparation method thereof |
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| CN108779019A (en) * | 2016-02-19 | 2018-11-09 | 费罗公司 | Sintering auxiliary glass for machinable phyllosilicate based structures |
| CN110040965A (en) * | 2019-03-29 | 2019-07-23 | 太原理工大学 | A kind of machinable ceramic material and preparation method thereof |
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| RU2142437C1 (en) * | 1997-07-16 | 1999-12-10 | Волгоградский инженерный центр "Ресурс" | Charge material for manufacturing glass ceramics |
| CN1314318A (en) * | 2000-03-20 | 2001-09-26 | 许淑惠 | Glass crystal brick as decorative building material made of broken glass and its producing method |
| CN1568291A (en) * | 2001-10-18 | 2005-01-19 | 迈克尔·J·豪恩 | Ceramic products, raw batch formulas and method |
| KR20030079097A (en) * | 2002-04-01 | 2003-10-10 | 윤연흠 | Production of glass-ceramics from waste glass and waste shell |
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| CN1915878B (en) * | 2006-09-05 | 2010-09-01 | 山东建筑大学材料科学研究所 | Method for producing color glass ceramic by using sludge of concrete |
| CN101844869A (en) * | 2010-05-24 | 2010-09-29 | 大连交通大学 | Method for preparing fluorine amphibole glass ceramic by using reactive crystallization-sintering method |
| CN101844869B (en) * | 2010-05-24 | 2012-07-04 | 大连交通大学 | Method for preparing fluorine amphibole glass ceramic by using reactive crystallization-sintering method |
| CN102617115A (en) * | 2011-01-28 | 2012-08-01 | 吕宝林 | Composition and method for smelting fluorophlogopite ceramic, and fluorophlogopite ceramic prepared from composition |
| 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 |
| CN102344251A (en) * | 2011-07-20 | 2012-02-08 | 大连交通大学 | Preparation method for lepidolite glass ceramic |
| CN104250067A (en) * | 2013-06-28 | 2014-12-31 | 中国地质大学（北京） | Method for preparation of machinable mica glass ceramic insulating material from waste glass and phlogopite |
| CN104250067B (en) * | 2013-06-28 | 2018-04-13 | 中国地质大学（北京） | A kind of method for preparing machinability mica glass-ceramics insulating materials using cullet and phlogopite |
| CN104973787A (en) * | 2015-06-10 | 2015-10-14 | 安徽省德邦瓷业有限公司 | Ageing-resistant glass ceramic disc and preparation method thereof |
| CN108779019A (en) * | 2016-02-19 | 2018-11-09 | 费罗公司 | Sintering auxiliary glass for machinable phyllosilicate based structures |
| CN108779019B (en) * | 2016-02-19 | 2021-06-04 | 费罗公司 | Sintering aid glass for machinable phyllosilicate-based structures |
| CN105906212A (en) * | 2016-04-21 | 2016-08-31 | 中南大学 | Mica-based glass ceramic and preparation method thereof |
| CN105906212B (en) * | 2016-04-21 | 2018-11-09 | 中南大学 | A kind of mica-based glass ceramics and preparation method thereof |
| CN106380080B (en) * | 2016-08-29 | 2019-02-01 | 中国建筑材料科学研究总院 | A kind of ion enhancing processable ceramic and preparation method thereof |
| CN106380080A (en) * | 2016-08-29 | 2017-02-08 | 中国建筑材料科学研究总院 | Ion-enhanced workable ceramics and preparation method thereof |
| CN110040965A (en) * | 2019-03-29 | 2019-07-23 | 太原理工大学 | A kind of machinable ceramic material and preparation method thereof |
| CN110040965B (en) * | 2019-03-29 | 2021-07-30 | 太原理工大学 | Machinable ceramic material and preparation method thereof |
| CN111253777A (en) * | 2020-01-20 | 2020-06-09 | 大连交通大学 | Ceramic pigment composition, black glass ceramic pigment, glass ceramic and preparation method thereof |
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