CN103819095A - Low-density foam glass and preparation method thereof - Google Patents
Low-density foam glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-density foam glass and a preparation method thereof. The low-density foam glass is characterized in that glass dust, carbon black, antimony trioxide, borax, titanium dioxide and a fluidizing agent are used as raw materials. The volume density of the foam glass prepared by the method is less than 140 Kg/m3; both the compression strength and the breaking strength are larger than 0.3 MPa, and the volume water absorption is less than 0.5%; at the room temperature, the heat conductivity is less than 0.065W/(m.K); the prepared foam glass has the advantages of light weight, high strength, small heat conductivity, moisture absorption resistance, good cold resisting property, corrosion resistance, wide use temperature, easiness in processing and the like, and can be used as a low-temperature insulating material or a heat insulating material for building interior and exterior walls.
Description
Technical field
The present invention relates to a kind of foam glass product, be specifically related to a kind of low density foam glass and preparation method thereof, belong to heat-insulating heat-preserving material technical field.
Background technology
Building material industry association has issued " 2010 building energy conservation target and the year two thousand twenty building energy conservation far-seeing plan target ".Because the power loss 50% of Chinese house house is in body of wall consumption, therefore urgently need carry out modernization overlay to external wall.Although typical organic heat insulating material for external such as molded polystyrene porous plastics (EPS), extrusion molding polystyrene polyfoam (XPS), rigid urethane foam (PU) have the features such as intensity is good, quality is light, airtight, corrosion-resistant, anti-aging, price is low, it is the main lagging material adopting in current domestic construction engineering, but the fire of high-rise building of sending out repeatly has in the recent period caused the query of various circles of society to these organic flammable heat insulating material for external, research and development green energy conservation, safe and reliable architecture of high quality lagging material become the active demand of the whole society.
According to the combustionproperty difference of material, material of construction has been carried out classification by China's national standard.Now conventional organic external-wall heat-insulation material all belongs to combustible matl, not only can bring great disaster hidden-trouble, and can discharge a large amount of toxic smogs when these organic materialss burnings, and personnel escape is brought to very big obstacle.The fire disaster accident that Chinese Central Television's new address BeiPeiLou fire in 2009, " 11.15 " Jing'an District, Shanghai wildfire in 2010, Shenyang feudal dynasty ten thousand February 3 in 2011 prosperous International Building fire contour level architecture exterior wall insulating materials cause, cause great society and politics impact, built inflammable flammable heat insulating material for external and caused the extensive concern of various circles of society.
Therefore, accelerate the research and development process of uninflammability external-wall heat-insulation material, accelerate the paces of its commercial application, meet the great demand of China's fire safety, have important practical significance.Multicellular glass is the porous glass material that a kind of inside is full of countless even bubbles, has many premium propertiess such as density is low, intensity is high, thermal conductivity is little.Organicly compare with inorganic heat insulation material with similar, the intensity of multicellular glass, weather resistance, water absorbing properties etc. all have obvious advantage, and shapeliness in addition, can meet the requirement of external thermal insulation system completely, therefore tool researching value.At present, multicellular glass has been put into the building material catalogue that state key is promoted and developed.Foam glass building heat insulation material has been incorporated into building end face and external wall outer insulation building standard atlas, for multicellular glass is laid a good foundation in the application in building thermal-insulation energy-saving field.
Multicellular glass becomes current study hotspot as the exploration of external-wall heat-insulation material.The volume density of product is to embody foamed glass foaming quality parameter the most intuitively, is also the performance index that product is focused on while applying as external-wall heat-insulation material most.Be limited to state of the art, the single line throughput of current multicellular glass is less, and technique, technology, equipment are relatively backward.Current disclosed data demonstration, the density optimum level of the multicellular glass of development is now: 145-175kg/m3, mean density is 160kg/m3.Research and development volume density becomes active demand lower than the multicellular glass of 140kg/m3.
Summary of the invention
Main purpose of the present invention is that a kind of volume density of invention is lower than 140kg/m
3good quality froth glass with and preparation method thereof.
Technical solution problem of the present invention, adopts following technical scheme:
Low density foam glass of the present invention, its feature is: described low density foam glass is take glass powder, carbon black, antimonous oxide, borax, titanium dioxide and liquid agent as starting material.
Low density foam glass of the present invention, its feature is also: the weight percent of each raw material is:
Preferably, the particle size range of described glass powder is 140-200 order; The particle diameter of described carbon black, antimonous oxide, borax, titanium dioxide and liquid agent is not more than 200 orders.
Preferably, the formation of the each compositions in weight percentage of described liquid agent is:
Preferably, described thickening polymer is selected from polyacrylic acid derivative, polyacrylamide derivative, ether of cellulose, polyphenylene oxide or polyalkylene glycol fatty acid ester.
The preparation method of low density foam glass of the present invention, its feature is: take ball mill or mixing machine that glass powder, carbon black, antimonous oxide, borax, titanium dioxide and liquid agent are mixed, obtain compound; On shaking table, described compound is poured in mould, made by vibration that compound is closely knit to be uniformly distributed, then put into stove and fire, obtain described multicellular glass.
Preferably, the condition of described vibration is: vibrational frequency is 50HZ, and amplitude is 5mm, and direction of vibration is at vertical and horizontal direction vibration, time of vibration 2～5s.
Preferably, the condition of firing described in is: rise to 350-450 ℃ from room temperature with 5-8 ℃/min temperature rise rate, insulation 20-30min; Rise to 750-850 ℃ with 10-20 ℃/min temperature rise rate again, insulation 20-30min; Be cooled to 550～650 ℃ with the rate of temperature fall of 15～20 ℃/min again, insulation 20～30min; Then be down to room temperature with the rate of temperature fall of 0.2～2 ℃/min.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the multicellular glass volume density that method of the present invention is prepared is lower than 140kg/m
3; Ultimate compression strength and folding strength are all greater than 0.3MPa; Volume water absorption rate is less than 0.5%; Under room temperature, thermal conductivity is less than 0.065W/ (m.K), and these goods reach industry gold standard;
2, from environment protection angle, the raw material that the present invention produces multicellular glass is to utilize various scrap glasses, belong to comprehensive utilization of waste materials, do not cause environmental pollution and ecological damage, the product of producing has significant environmental benefit, and can be a large amount of soil, fuel, the manpower and materials of country's saving, and can not produce detrimentally affect to environment in production and use procedure, production process does not produce " three wastes ", is a kind of green energy conservation product;
3, architecture exterior wall insulating materials market outlook are wide, therefore the demand to architecture exterior wall insulating materials towards country, development low density foam glass architecture wall heat insulation material and the technology that forms a complete production network, in solving the higher fire hazard problem of current external-wall heat-insulation material existence, can realize the double goal such as building energy conservation and resource reutilization;
4, the multicellular glass that prepared by the present invention has light weight, intensity is high, thermal conductivity is little, non-hygroscopic, frost resistance good, corrosion-resistant, use temperature wide, be easy to the advantages such as processing, can be used as low temperature lagging material or Discussion on architecture metope lagging material.
Specific embodiment
The present invention takes ball mill or V-Mixer that glass powder, carbon black, antimonous oxide, borax, titanium dioxide and liquid agent are mixed, and obtains compound; On shaking table, described compound is poured in mould, made by vibration that compound is closely knit to be uniformly distributed, then put into stove and fire, obtain described multicellular glass.
In order to analyse in depth method of the present invention, do following research:
1. formulation selection
1.1 major ingredients: glass powder
Glass powder is the main raw material of manufacturing multicellular glass, and quality and the production process system of its performance quality on product has important impact.SiO
2be the main component of glass, it is fused into the liquid with certain viscosity in the time heating up, and is beneficial to the bubble that storage foam material produces, and solidifies and bubble is wrapped up, thereby form multicellular glass when cooling.Granularity as raw-material glass powder is moderate, if particle is excessively thick, swelling property is poor, forms thick multicellular glass; Otherwise swelling property is good, but be unfavorable for the even mixing of whipping agent; Experimental results demonstrate best results when the granularity of glass powder can be all by 140-200 mesh sieve (particle diameter be 70-100 micron).
1.2 whipping agents: carbon black
Glass is conducive to the melt temperature of foaming generally at 700～900 ℃, and selected whipping agent should be able to foam in this temperature range, and the bubble in multicellular glass is independently, and whipping agent total amount and single particle whipping agent should adapt with it.Preferred according to many experiments, as whipping agent, can manufacture the low density foam glass of the thin spilehole structure of remaining silent uniformly of wall-forming with pure carbon.Carbon black is the Typical Representative of oxidized form whipping agent, and carbon black, except having whipping agent effect, also has the effect of stablizer.In the time having unreacted carbon black, because the chemical affinity of it and liquid glass is less, soaked by glass hardly, carbon black fine particle concentrates on the interface of liquid phase, and the interfacial energy on phase interface is reduced, thereby is conducive to the stable of crafters.Carbon is as whipping agent, is to take oxysome (M based on some in carbon and glass
xo
y), oxygen, moisture etc. carries out oxidizing reaction, produces a large amount of gas, gas mainly contains CO
2, CO, H
2deng, its chemical equation is as follows:
C+O
2=CO
2↑ CO
2+C=2CO↑
C+H
2O=H
2↑+CO↑ yC+MxOy=xM(x/y)O+yCO↑
1.3 additive
Liquid agent:
Because the decomposition temperature of carbon black is much smaller than glass melting temperature, at admixtion, not before densified sintering product, gas produces, and overflows by hole between glass particle, causes bubble rate to reduce; And due to the heat insulating function of batch particle gap entrap bubble, cause the thermal conductivity of admixtion unbalanced in all directions, and generate Air Bubble Size and differ, disperse inhomogeneously, have a strong impact on foaming quality.Therefore need to add appropriate liquid agent, its effect is: 1 strengthens powder fluidity; 2 suppress carbon granule reunites and flocculates; 3 that whipping agent is easy to is dispersed.
Fusing assistant: borax
Because the decomposition temperature of carbon black is much smaller than glass melting temperature, when foaming, gas is easily never overflowed in fine and close base substrate.Only in the time that gas produces in a large number, admixtion has softened into glassy phase and has wrapped the gas of generation, just can obtain the multicellular glass that foaming quality is good.Therefore, must in admixtion, add a certain amount of fusing assistant to adjust the surface properties of glass particle, reduce the viscosity of glass, make glass be easy to melting.In the raw material of manufacturing multicellular glass, adding appropriate promotor is very important for making low density closed-cell foam glass.The introducing of fusing assistant can improve physicochemical property and the production process system of goods, can reduce blowing temperature, increases blowing temperature scope, makes to be communicated with pore and reduces yield rate raising.
Suds-stabilizing agent: titanium dioxide
Be used for preventing that small bubbles from mutually combining forms communicating aperture or break, thus stabilise bubbles structure.Conventionally there is polar covalent bond, semi-metal covalent linkage or the large transition metal of field intensity, can in glass, form [MO with oxygen
4] tetrahedral structure, can be used as suds-stabilizing agent.
Foamed promoter: antimonous oxide
Claim again vaporized chemical, by pyrolytic decomposition releasing oxygen, to promote whipping agent foaming, improve the foaming and intumescing ability of glass.Conventional foamed promoter is antimonous oxide, and antimonous oxide at low temperatures can be oxidized, reduces the oxygenolysis of carbon dust, and the next releasing oxygen of high temperature promotes foaming.
Experimental results demonstrate best results when the granularity of whipping agent carbon black and other additives can be all by 200 mesh sieves (particle diameter be for being not more than 70 microns).
2. process choice
The mixing of 2.1 raw materials
Particle diameter is not more than 200 object carbon blacks and other each additives and particle diameter 140-200 object glass powder must full and uniform mixing, therefore adopts ball mill or mixing machine, can mix so more even.
2.2 forming method
If directly compound is poured in mould, compound can random accumulation in mould, its surface irregularity, and the middle space varying in size that exists, this is foam glass product performance of impact preparation greatly.So mould must be placed on shaking table, regulating the vibrational frequency of shaking table is 50HZ, and amplitude is 5mm, in vertical and horizontal direction vibration, time of vibration 2～5s pours compound in mould into simultaneously, under oscillating action, compound is can be in mould closely knit and distribute uniformly.
2.3 sintering procedure
Multicellular glass is the heterogeneous system that the gas of balance, solid two-phase form.Low density foam glass, its gas phase accounts for the more than 90% of cubic capacity.In the forming process of foam bubbles, the viscosity of melten glass liquid is gentle, the surface tension at liquid interface has important effect.Glass melt has enough large viscosity can stop breaking of bubble wall film, prevents communicating aperture, and surface tension is little to be conducive to promote walls attenuation be beneficial to the density that reduces multicellular glass.The viscosity of glass melt and surface tension are all the functions of temperature, can be by regulating the height of blowing temperature, and the length of foamed time control effectively.The important step that multicellular glass is produced so formulate rational firing temperature system.In order to make powder even foaming, if rate of heating is preferably controlled, heat-up rate is too fast within the specific limits, and not only foaming size is uneven, and on also there being impact the work-ing life of metal die.The sintering technology of multicellular glass is roughly divided into a stage preheating, foaming, stable, annealing.
A, preheating: rise to 350-450 ℃ from room temperature with the temperature rise rate of 5-8 ℃/min, insulation 20-30min.
Because the thermal conductivity of the compound of powdery is smaller, directly enter firing furnace and can cause the decomposition oxidation of top layer whipping agent and the too early melting of Watch glass powder, make compound ectonexine temperature head compared with large and cause foaming inhomogeneous.Therefore must before burning till, carry out preheating, preheating temperature should, below the decomposition temperature of whipping agent, be generally 350-450 ℃.Be generally 20-30min warm up time.Preheating temperature is unsuitable too high, and warm up time is also unsuitable long.All can make too high preheating temperature and long warm up time the whipping agent on top layer decompose prematurely oxidation, make product surface porcelain, even make goods foaming difficulty and density increase.Warm is mainly chemically-bonded water, planar water and the free-water of taking off in admixtion.
B, foaming: the temperature rise rate with 10-20 ℃/min rises to 750-850 ℃, insulation 20-30min.
Compound after preheating is heated rapidly, and the object being rapidly heated is the decomposition that prevents that whipping agent is too much, and the gas phase that makes along with the intensification of base substrate sharply to increase is wrapped in base substrate and do not overflow, thereby can obtain more gas phase.But can not take too fast temperature rise rate, because there has been bubble formation the admixtion inside of melting, heat conductivility variation, heats up and can cause too soon material non-uniform temperature everywhere, causes foaming uneven, affects the air hole structure of material.After being warmed up to blowing temperature, need to be incubated for some time.Within the scope of the blowing temperature of multicellular glass, blowing temperature can be got high value also can get low value, as long as choose corresponding foamed time, just can obtain needed foam glass product.The high required foamed time of blowing temperature is just shorter, and the low required foamed time of blowing temperature is just longer.But blowing temperature is too low, the long meeting of foamed time makes the surperficial porcelain of goods, is unfavorable for making low density foam glass.Blowing temperature is too high, and the too short meeting of foamed time makes the inside and outside bubble diameter inequality of goods, and the bubble aperture of surrounding is larger, and blowing temperature to get over the high-foaming time shorter, this aperture difference is also larger.Generally more stable with middle temperature foaming, bubble diameter is more even, and the defects such as bulla, communicating aperture, depression are fewer, and the yield rate of goods is also higher.
C, surely bubble: be cooled to 550～650 ℃ with the rate of temperature fall of 15～20 ℃/min, insulation 20～30min.
In the time that foaming finishes, rapidly sample is cooled to 550-650 ℃ of left and right, it is fast that speed of cooling is wanted, generally at 15-20 ℃/min.Its objective is the air hole structure of generation is fixed up rapidly.Because sample is cooling rapidly, will produce stress, for eliminating stress, the multicellular glass after foaming is cooled to annealing beginning temperature to be incubated.After multicellular glass after foaming is cooling, temperature-fall period will inevitably be expanded to center from surrounding, the surrounding top layer of goods can form very soon one deck cured layer and expand to center gradually, start insulation in this temperature, can slow down cured layer to the propagation rate at center, make goods inside still have certain continuation foamed time, overcome temperature head and time difference in foaming process, make the outer compensation that the contraction that causes obtains of solidifying simultaneously, can reduce significantly the defect such as depression, crack of goods.
D, annealing: the rate of temperature fall with 0.2～2 ℃/min is down to room temperature.
Then turn off power supply and naturally cool to room temperature.The annealing cool speed of multicellular glass is not only relevant with chemical constitution, the thickness of goods, also relevant with the structure of goods, density, thermal expansivity etc.Because the thermal conductivity of multicellular glass is little, its annealing cool speed is much slower than the annealing cool speed of simple glass, and total cool down time is more than 24 hours.The annealing cool speed of multicellular glass generally should be slower with the Xu Lengwei master's, particularly low-temperature zone of constant speed of cooling speed of cooling.Speed of cooling can make the stress of goods increase soon, strength decreased, and the decrease in yield of product, the while also can make the post-treatment degradation of multicellular glass.
Adopt the foam glass product property detection method of the building material industry standard JC/T647-2005 of the People's Republic of China (PRC) to test, the overall performance of the multicellular glass of preparing by present method is: volume density 123-136kg/m
3; Ultimate compression strength 0.35-0.46Mpa; Folding strength 0.34-0.42MPa; Volume water absorption rate 0.3-0.48%; Thermal conductivity 0.058-0.064W/ (m.K) under room temperature.These goods reach industry gold standard.
Embodiment 1
First, take particle diameter 200-240 object, account for respectively the carbon black of gross weight 0.5%, 1% antimonous oxide, 1% borax, 1% titanium dioxide, 0.1% liquid agent (polyoxyethylene glycol 30%; Diethylene glycol monobutyl ether 50%; Polysaccharide 10%; Ether of cellulose 10%) and particle size range 140-200 order, account for the glass powder of gross weight 96.4%; Then, take mixing machine that each component is mixed; Then, on shaking table, compound is poured in mould (450mm × 350mm × 100mm), vibration 2s, make it closely knit and uniformly distribute; Finally, mould is put into stove, rise to 400 ℃ from room temperature with 5 ℃/min temperature rise rate, insulation 25min; Rise to 800 ℃ with 20 ℃/min temperature rise rate again, insulation 25min; Be cooled to 600 ℃ with the rate of temperature fall of 20 ℃/min again, insulation 30min; Then be cooled to room temperature with the rate of temperature fall of 1 ℃/min.Complete foam glass product.The parameters of the multicellular glass of preparing by present method is respectively: volume density 125kg/m
3; Ultimate compression strength 0.35Mpa; Folding strength 0.34MPa; Volume water absorption rate 0.39%; Thermal conductivity 0.061W/ (m.K) under room temperature.These goods reach industry standard.
Embodiment 2
First, take particle diameter 200-240 object, account for respectively the carbon black of gross weight 0.8%, 1.5% antimonous oxide, 1% borax, 1% titanium dioxide, 0.1% liquid agent (polyoxyethylene glycol 40%; Diethylene glycol monobutyl ether 40%; Polysaccharide 15%; Polyphenylene oxide 5%) and particle size range 140-200 order, account for the glass powder of gross weight 95.6%; Then, take ball mill that each component is mixed; Then, on shaking table, compound is poured in mould (450mm × 350mm × 100mm), vibration 3s, make it closely knit and uniformly distribute; Finally, mould is put into stove, rise to 400 ℃ from room temperature with 6 ℃/min temperature rise rate, insulation 25min; Rise to 800 ℃ with 20 ℃/min temperature rise rate again, insulation 25min; Be cooled to 600 ℃ with the rate of temperature fall of 15 ℃/min again, insulation 30min; Then be cooled to room temperature with the rate of temperature fall of 0.5 ℃/min.Complete foam glass product.The parameters of the multicellular glass of preparing by present method is respectively: volume density 128kg/m
3; Ultimate compression strength 0.37Mpa; Folding strength 0.35MPa; Volume water absorption rate 0.42%; Thermal conductivity 0.063W/ (m.K) under room temperature.These goods reach industry standard.
Embodiment 3
First, take particle diameter 200-240 object, account for respectively the carbon black of gross weight 1%, 2% antimonous oxide, 0.8% borax, 0.8% titanium dioxide, 0.1% liquid agent (polyoxyethylene glycol 50%; Diethylene glycol monobutyl ether 20%; Polysaccharide 20%; Polyalkylene glycol fatty acid ester 10%) and particle size range 140-200 order, account for the glass powder of gross weight 95.3%; Then, take mixing machine that each component is mixed; Then, on shaking table, compound is poured in mould (450mm × 350mm × 100mm), vibration 5s, make it closely knit and uniformly distribute; Finally, mould is put into stove, rise to 400 ℃ from room temperature with 7 ℃/min temperature rise rate, insulation 30min; Rise to 800 ℃ with 15 ℃/min temperature rise rate again, insulation 25min; Be cooled to 600 ℃ with the rate of temperature fall of 20 ℃/min again, insulation 30min; Then be cooled to room temperature with the rate of temperature fall of 2 ℃/min.Complete foam glass product.The parameters of the multicellular glass of preparing by present method is respectively: volume density 135kg/m
3; Ultimate compression strength 0.45Mpa; Folding strength 0.41MPa; Volume water absorption rate 0.47%; Thermal conductivity 0.064W/ (m.K) under room temperature.These goods reach industry standard.
Claims (8)
1. a low density foam glass, is characterized in that: described low density foam glass is take glass powder, carbon black, antimonous oxide, borax, titanium dioxide and liquid agent as starting material.
2. low density foam glass according to claim 1, is characterized in that: the weight percent of each raw material is:
3. low density foam glass according to claim 1 and 2, is characterized in that: the particle size range of described glass powder is 140-200 order; The particle diameter of described carbon black, antimonous oxide, borax, titanium dioxide and liquid agent is not more than 200 orders.
4. low density foam glass according to claim 1 and 2, is characterized in that: the formation of the each compositions in weight percentage of described liquid agent is:
5. low density foam glass according to claim 4, is characterized in that: described thickening polymer is selected from polyacrylic acid derivative, polyacrylamide derivative, ether of cellulose, polyphenylene oxide or polyalkylene glycol fatty acid ester.
6. a preparation method for low density foam glass described in claim 1 or 2, is characterized in that: take ball mill or mixing machine that glass powder, carbon black, antimonous oxide, borax, titanium dioxide and liquid agent are mixed, obtain compound; On shaking table, described compound is poured in mould, made by vibration that compound is closely knit to be uniformly distributed, then put into stove and fire, obtain described multicellular glass.
7. preparation method according to claim 6, is characterized in that: the condition of described vibration is: vibrational frequency is 50HZ, and amplitude is 5mm, and direction of vibration is in vertical and horizontal direction vibration.
8. preparation method according to claim 6, is characterized in that: described in the condition fired be: rise to 350-450 ℃ from room temperature with 5-8 ℃/min temperature rise rate, insulation 20-30min; Rise to 750-850 ℃ with 10-20 ℃/min temperature rise rate again, insulation 20-30min; Be cooled to 550～650 ℃ with the rate of temperature fall of 15～20 ℃/min again, insulation 20～30min; Then be down to room temperature with the rate of temperature fall of 0.2～2 ℃/min.
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| CN108840572A (en) * | 2018-07-16 | 2018-11-20 | 江苏省苏安能节能建材科技有限公司 | A kind of low cost foam glass thermal insulation material and its preparation and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262005A (en) * | 2014-09-28 | 2015-01-07 | 陕西科技大学 | Method for preparing light porous particle controlled release fertilizer |
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| CN108840572A (en) * | 2018-07-16 | 2018-11-20 | 江苏省苏安能节能建材科技有限公司 | A kind of low cost foam glass thermal insulation material and its preparation and application |
| CN109608041A (en) * | 2018-12-29 | 2019-04-12 | 河南万里绝热材料股份有限公司 | A kind of foam glass and preparation method thereof of mixing scrap glass preparation |
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Application publication date: 20140528 |