CN101113076A - Microcrystal foam glass prepared by kerosene shale ash and manufacturing method thereof - Google Patents

Microcrystal foam glass prepared by kerosene shale ash and manufacturing method thereof Download PDF

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Publication number
CN101113076A
CN101113076A CNA2007100119735A CN200710011973A CN101113076A CN 101113076 A CN101113076 A CN 101113076A CN A2007100119735 A CNA2007100119735 A CN A2007100119735A CN 200710011973 A CN200710011973 A CN 200710011973A CN 101113076 A CN101113076 A CN 101113076A
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China
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glass
shale ash
ash
foam glass
kerosene shale
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CN100582042C (en
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薛向欣
冯宗玉
李勇
杨合
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Northeastern University China
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Northeastern University China
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Abstract

The invention relates to a microcrystalline foam glass made by oil shale ash and a preparation method thereof. The oil shale ash is used as main material. The basic glass is made by adding a certain quantity of calcium carbonate, basic magnesium carbonate, borax and sodium carbonate to the main material, then adding foaming agent, foam stabilizer, fluxing agent. By adopting powder firing technique, the microcrystalline foam glass is made. The surface volume consistency of the glass is 875-1030 kg.m-3; absorbing capability is 8-15 percent; compressive strength is 11-23 MPa; bending strength is 10-17MPa; and heat conductive coefficient is 0.21- 0.32w(m.k)-1.The producing steps comprise the following techniques that first-time material proportioning; high temperature melting; basic glass making; second-time material proportioning; foaming; foam stabilizing; annealing, etc. The microcrystalline foam glass is a novel multi-functional material, which has remarkable meaning on improvement of the added value of oil shale rock resources and on environment protection.

Description

Prepare crystallite foam glass and manufacture method thereof with kerosene shale ash
Technical field
The present invention relates to a kind of is the crystallite foam glass and the manufacture method of main raw material preparation with the kerosene shale ash.
Background technology
Crystallite foam glass is a kind of novel multifunctional material.Be mainly used in the bearing wall of (1) buildings; (2) cryogenic piping, equipment, container and storage tank; (3) deep fat and heated bitumen storage tank; (4) petrochemical complex, sulfuration production process; (5) fluid heat-exchange system; (6) extensive fields such as the sound insulation of compressor, Ventilator Room and sound-absorbing wall.
Crystallite foam glass be a kind of be main raw material with cullet, flyash, nonmetalliferous ore etc., add whipping agent, nucleator and admixture etc., mix the formation admixtion after crushed, then admixtion is put in the mould and in electric furnace, heats, through preheating, sintering, foaming, surely steep and novel porous microcrystal glass material that technology such as annealing is made.
Since the general multicellular glass height of strength ratio of crystallite foam glass, the advantage that the volume to weight ratio devitrified glass is little.In recent years, selection, performance, application and the blowing temperature of the preparation technology of crystallite foam glass, raw material are determined etc. that all there is research the aspect.Chen Kerong etc. have prepared foamed glass ceramic material for wall with glass powder, flyash and nonmetalliferous ore; Wang Lijius etc. are basic material with cullet and light ceramic, have prepared novel crystallite foam glass material; Guo Hongwei etc. are main raw material with the cullet, as whipping agent, as nucleator, have prepared crystallite foam glass with Vanadium Pentoxide in FLAKES with carbon dust.Above technological line all is to be main raw material with the cullet, and is less relatively to the utilization ratio of non-metallic minerals.
Resinous shale is the organic mineral products of a kind of high-ash solid combustible.China's resinous shale finds out that stock number is 329.89 hundred million t, occupies the 4th in the world, mainly is distributed in northeast and ALFISOL IN CENTRAL.Refine a large amount of lime-ash of meeting generation in shale oil and the oil shale combustion process at resinous shale, need take a large amount of soils and cause problems such as serious environmental pollution, therefore how improving the comprehensive utilization ratio of resinous shale lime-ash, improve the added value of oil shale resources, is the technical problem that needs to be resolved hurrily.
Summary of the invention
At crystallite foam glass preparation in the prior art, non-metallic minerals is the low present situation of industrial residue utilization rate especially, the invention provides a kind ofly to prepare crystallite foam glass and manufacture method thereof with kerosene shale ash.
The present invention is a main raw material with the kerosene shale ash, adds an amount of chemical reagent, adopts powder method firing technology single stage method (being that one step foaming just obtains crystallite foam glass) to prepare well behaved crystallite foam glass.Below be the kerosene shale ash chemical constitution (massfraction %) of the main shale oil plant of China:
SiO 2 Al 2O 3 Fe 2O 3 CaO MgO K 2O+Na 2O
55~65 18~26 7~11 0.5~1.5 1~2 0.7~3
Preparation technology's flow process of the present invention:
Once batching → high temperature melting → parent glass → second batch → foaming → surely steep and annealing → blank → cutting → finished product.Processing step of the present invention:
1. batching once: according to the chemical composition analysis of kerosene shale ash and to the requirement of product, by weight batching: kerosene shale ash 70~80%, lime carbonate 10~15%, magnesium basic carbonate 3~5%, borax 4~6%, yellow soda ash 3~5%;
2. high temperature melting: with various raw materials after accurate weighing in ball mill uniform mixing, join in the high alumina crucible and put in the Si-Mo rod resistance furnace, at 1250~1300 ℃ of following fusion 90~120min;
3. parent glass preparation: glass is melted body pour into rapidly in the tap water, shrend becomes the glass particle of 0.074~0.2mm, in drying baker in 100.Dry 30min puts into ball mill with exsiccant shrend glass particle, and ball milling becomes the glass powder of granularity less than 0.074mm;
4. second batch: by weight batching: set 100 parts in glass powder, add corresponding whipping agent lime carbonate 2~5%, suds-stabilizing agent sodium phosphate 3~8%, fusing assistant borax 2~5%;
5. foaming: after admixtion mixed in ball mill, join in the high alumina crucible and put into the Si-Mo rod resistance furnace, be warmed up to 1070~1090 ℃, insulation 15~25min with the temperature rise rate of 10~15 ℃/min;
6. surely steep and anneal: when foaming finishes, cool to 600 ℃, insulation 15~25min with the speed of 15~25 ℃/min.Furnace cooling is to room temperature then;
Detect: prepared blank, detect after cutting into the crystallite foam glass finished product.Crystallite foam glass apparent bulk density 875~1030kgm -3, water-absorbent 8~15%, ultimate compression strength 11~23MPa, folding strength 10~17MPa, thermal conductivity 0.21~0.32w (mk) -1
The invention provides the novel method of oil page or leaf charcoal ash preparation crystallite foam glass, can improve environment by the reasonable use kerosene shale ash.
Embodiment
Embodiment 1
1. once prepare burden: by weight preparing burden: kerosene shale ash 70%, lime carbonate 15%, magnesium basic carbonate 5%, borax 6%, yellow soda ash 4%;
2. high temperature melting: accurately behind the various raw materials of weighing, uniform mixing in ball mill joins in the high alumina crucible, 1250 ℃ of fusion 90min in the Si-Mo rod resistance furnace;
3. parent glass preparation: glass is melted body pour into rapidly in the tap water, shrend becomes the glass particle of 0.074~0.2mm, in drying baker in 100 ℃ of dry 30min; Exsiccant glass particle ball milling is become the powder of granularity less than 0.074mm;
4. second batch: by weight batching: set 100 parts in glass powder, add whipping agent lime carbonate 2%, suds-stabilizing agent sodium phosphate 4%, fusing assistant borax 3%;
5. foaming: after admixtion mixed in ball mill, join in the high alumina crucible and put into the Si-Mo rod resistance furnace, be incubated 20min after being warmed up to 1090 ℃ with the temperature rise rate of 10 ℃/min;
6. surely steep and anneal: when foaming finishes, cool to 600 ℃, insulation 15min with the speed of 20 ℃/min.Furnace cooling is to room temperature then.
The prepared crystallite foam glass performance index of above-mentioned technology are: apparent bulk density 1030kgm -3, water-absorbent 12%, ultimate compression strength 15MPa, folding strength 12MPa, thermal conductivity 0.32w (mk) -1
Embodiment 2
1. once prepare burden: by weight preparing burden: kerosene shale ash 78%, lime carbonate 10%, magnesium basic carbonate 3%, borax 5%, yellow soda ash 4%;
2. high temperature melting: with various raw materials after accurate weighing in ball mill uniform mixing, join in the high alumina crucible, and put in the electric furnace in 1250 ℃ of fusion 110min;
3. parent glass preparation: molten mass is poured into rapidly in the tap water, and shrend becomes the glass particle of 0.074~0.2mm, and behind 100 ℃ of dry 30min, ball milling becomes the glass powder of granularity less than 0.074mm in drying baker;
4. second batch: by weight batching: set 100 parts in glass powder, add lime carbonate 4%, sodium phosphate 6%, borax 4%;
5. foaming: after with ball mill admixtion being mixed, join the high alumina crucible after, put in the Si-Mo rod resistance furnace, be warmed up to 1080 ℃, insulation 15min with the temperature rise rate of 12 ℃/min;
6. surely steep and anneal: when foaming finishes, cool to 600 ℃, insulation 20min with the speed of 18/min.Furnace cooling is to room temperature then.
The prepared crystallite foam glass performance index of above-mentioned technology are: apparent bulk density 957kgm -3, water-absorbent 10%, ultimate compression strength 19MPa, folding strength 14MPa, thermal conductivity 0.28w (mk) -1
Embodiment 3
1. once prepare burden: by weight preparing burden: kerosene shale ash 78%, lime carbonate 10%, magnesium basic carbonate 3%, borax 4%, yellow soda ash 5%;
2. high temperature melting: various raw materials through accurately mixing in ball mill after the weighing, are joined in the high alumina crucible and put in the electric furnace, at 1250 ℃ of following fusion 100min;
3. parent glass preparation: glass is melted body pour into rapidly in the tap water, shrend becomes the glass particle of 0.074~0.2mm, in drying baker in 100 ℃ of dry 30min; Exsiccant shrend glass particle ball milling is become the glass powder of granularity less than 0.074mm;
4. second batch: by weight batching: set 100 parts in glass powder, add corresponding whipping agent lime carbonate 3%, suds-stabilizing agent sodium phosphate 3%, fusing assistant borax 5%.
5. foaming: with ball mill with the admixtion uniform mixing after, join in the high alumina crucible, put into the Si-Mo rod resistance furnace and be warmed up to 1085 ℃, insulation 15min with the temperature rise rate of 12 ℃/min.
6. surely steep and anneal: when foaming finishes, cool to 600 ℃, insulation 20min with the speed of 15 ℃/min.Furnace cooling is to room temperature then.
The prepared crystallite foam glass performance index of above-mentioned technology are: apparent bulk density 911kgm -3, water-absorbent 8%, ultimate compression strength 23MPa, folding strength 17MPa, thermal conductivity 0.21w (mk) -1
Embodiment 4
1. once prepare burden: by weight preparing burden: kerosene shale ash 80%, lime carbonate 10%, magnesium basic carbonate 3%, borax 4%, yellow soda ash 3%;
2. high temperature melting: after the accurate weighing of raw material, uniform mixing in ball mill joins in the high alumina crucible and puts in the Si-Mo rod resistance furnace, at 1300 ℃ of following fusion 120min;
3. parent glass preparation: glass is melted body pour into rapidly in the tap water, shrend becomes the glass particle of 0.074~0.2mm, in drying baker in 100 ℃ of dry 30min; The exsiccant glass particle is put into ball mill, and ball milling becomes the glass powder of granularity less than 0.074mm;
4. second batch: by weight batching: set 100 parts in glass powder, add corresponding whipping agent lime carbonate 5%, suds-stabilizing agent sodium phosphate 8%, fusing assistant borax 2%.
5. foaming: admixtion behind the uniform mixing, is joined in the high alumina crucible in ball mill, and the temperature rise rate with 15 ℃/min in electric furnace is warmed up to 1070 ℃, insulation 25min.
6. surely steep and anneal: when foaming finishes, cool to 600 ℃, insulation 25min with the speed of 25 ℃/min.Furnace cooling is to room temperature then.
The prepared crystallite foam glass performance index of above-mentioned technology are: apparent bulk density 875kgm -3, water-absorbent 15%, ultimate compression strength 11MPa, folding strength 10MPa, thermal conductivity 0.23w (mk) -1

Claims (2)

1. a crystallite foam glass that utilizes the kerosene shale ash preparation is characterized in that with the kerosene shale ash being main raw material, adopts powder method to burn till, and its apparent bulk density is 875~1030kgm -3, water-absorbent 8~15%, ultimate compression strength 11~23MPa, folding strength 10~17MPa, thermal conductivity 0.21~0.32w (mk) -1
2. the preparation method of the described crystallite foam glass of claim 1 is characterized in that may further comprise the steps:
1) batching once: according to the chemical composition analysis of kerosene shale ash and to the requirement of product, by weight batching: kerosene shale ash 70~80%, lime carbonate 10~15%, magnesium basic carbonate 3~5%, borax 4~6%, yellow soda ash 3~5%;
2) high temperature melting: with various raw materials after accurate weighing in ball mill uniform mixing, join in the high alumina crucible and put in the Si-Mo rod resistance furnace, at 1250~1300 ℃ of following fusion 90~120min;
3) parent glass preparation: glass is melted body pour into rapidly in the tap water, shrend becomes the glass particle of 0.074~0.2mm, in drying baker in 100 ℃ of dry 30min; Exsiccant shrend glass particle is put into ball mill, and ball milling becomes the glass powder of granularity less than 0.074mm;
4) second batch: by weight preparing burden: set 100 parts in glass powder, add corresponding whipping agent lime carbonate 2~5%, suds-stabilizing agent sodium phosphate 3~8%, fusing assistant borax 2~5%;
5) foaming: after admixtion mixed in ball mill, join in the high alumina crucible and put into the Si-Mo rod resistance furnace, be warmed up to 1070~1090 ℃, insulation 15~25min with the temperature rise rate of 10~15 ℃/min;
6) surely steep and anneal: when foaming finishes, cool to 600 ℃ with the speed of 15~25 ℃/min, insulation 15~25min, furnace cooling is to room temperature then.
CN200710011973A 2007-07-05 2007-07-05 Microcrystal foam glass prepared by kerosene shale ash and manufacturing method thereof Expired - Fee Related CN100582042C (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838283A (en) * 2012-10-11 2012-12-26 南京师范大学 Method for producing foam microcrystal glass by utilizing composite industrial residue and product
CN103086587A (en) * 2013-02-22 2013-05-08 石河子大学 Preparation method of expanded vermiculite foam glass insulating material
CN103570245A (en) * 2012-07-25 2014-02-12 咸阳陶瓷研究设计院 Foam glass prepared from shale and manufacturing method thereof
CN104446362A (en) * 2014-12-08 2015-03-25 宁夏黑金科技有限公司 Sandstone-shale-produced material special for road, slope protection and canal as well as manufacturing method of material
CN104445958A (en) * 2014-11-18 2015-03-25 中国建筑材料科学研究总院 Fluorcanasite microcrystalline reinforced foam glass and preparation method thereof
CN104909546A (en) * 2015-06-05 2015-09-16 上海第二工业大学 Method for preparing micro-crystallographic foamed glass by using waste CRT (cathode ray tube) screen glass
CN105293907A (en) * 2015-10-16 2016-02-03 华南农业大学 Foam glass ceramics releasing anions and having far-infrared emission function and preparation method and application thereof
WO2018086514A1 (en) * 2016-11-08 2018-05-17 宁夏黑金科技有限公司 Production process for producing microcrystal foamed fireproof thermal insulation board from oily sludge residues

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103570245A (en) * 2012-07-25 2014-02-12 咸阳陶瓷研究设计院 Foam glass prepared from shale and manufacturing method thereof
CN102838283A (en) * 2012-10-11 2012-12-26 南京师范大学 Method for producing foam microcrystal glass by utilizing composite industrial residue and product
CN102838283B (en) * 2012-10-11 2014-12-17 南京师范大学 Method for producing foam microcrystal glass by utilizing composite industrial residue and product
CN103086587A (en) * 2013-02-22 2013-05-08 石河子大学 Preparation method of expanded vermiculite foam glass insulating material
CN103086587B (en) * 2013-02-22 2015-12-02 石河子大学 The preparation method of expanded vermiculite foam glass thermal insulation material
CN104445958A (en) * 2014-11-18 2015-03-25 中国建筑材料科学研究总院 Fluorcanasite microcrystalline reinforced foam glass and preparation method thereof
CN104445958B (en) * 2014-11-18 2017-01-18 中国建筑材料科学研究总院 Fluorcanasite microcrystalline reinforced foam glass and preparation method thereof
CN104446362A (en) * 2014-12-08 2015-03-25 宁夏黑金科技有限公司 Sandstone-shale-produced material special for road, slope protection and canal as well as manufacturing method of material
CN104909546A (en) * 2015-06-05 2015-09-16 上海第二工业大学 Method for preparing micro-crystallographic foamed glass by using waste CRT (cathode ray tube) screen glass
CN105293907A (en) * 2015-10-16 2016-02-03 华南农业大学 Foam glass ceramics releasing anions and having far-infrared emission function and preparation method and application thereof
CN105293907B (en) * 2015-10-16 2018-01-30 华南农业大学 Discharge anion and transmitting far-infrared functional foam pyroceram and its preparation method and application
WO2018086514A1 (en) * 2016-11-08 2018-05-17 宁夏黑金科技有限公司 Production process for producing microcrystal foamed fireproof thermal insulation board from oily sludge residues

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