CN102795780B - A kind of low temperature crystallite foam glass and preparation method thereof - Google Patents
A kind of low temperature crystallite foam glass and preparation method thereof Download PDFInfo
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- CN102795780B CN102795780B CN201210295629.4A CN201210295629A CN102795780B CN 102795780 B CN102795780 B CN 102795780B CN 201210295629 A CN201210295629 A CN 201210295629A CN 102795780 B CN102795780 B CN 102795780B
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Abstract
The present invention relates to a kind of low temperature crystallite foam glass and preparation method thereof, in this crystallite foam glass, the mol ratio of each main ingredient is: Na
2o (K
2and SiO O)
2mol ratio be 0.1 ~ 1.0:1, SiO
2with Al
2o
3mol ratio be 1.0 ~ 20:1, B
2o
3with SiO
2mol ratio be 0 ~ 0.2:1; Its preparation method comprises: water glass, reactive aggregate mix and stir by (1), add additive afterwards, obtain colloidal sol; (2) by aging for above-mentioned colloidal sol 1 ~ 7 day, then that the colloidal sol after aging is dry, obtained water ratio is the solid gel of 10% ~ 50%; (3) above-mentioned solid gel is smashed to pieces, load in mould, finally foam.Crystallite foam glass density of the present invention is low, and intensity is high, and thermal and insulating performance is good, long service life, and fire resistance is good, and preparation method of the present invention is simple to operate, reduces blowing temperature.
Description
Technical field
The invention belongs to crystallite foam glass and preparation field thereof, particularly a kind of low temperature crystallite foam glass and preparation method thereof.
Background technology
[2011] No. 65 official document regulations that public affairs disappear: 1, covil construction heat insulating material for external is included in the examination & verification of construction project design for fire protection, fire control acceptance and extent of tests of putting on record.Before new standard is issued, execution as strict as possible " covil construction outer heat preservation system and decoration of exterior wall fire prevention temporary provisions " (public logical No. [2009] 46, word) Article 2 regulation, covil construction heat insulating material for external employing combustionproperty is the material of A level.2, the fire supervision management of covil construction heat insulating material for external is strengthened.On March 15th, 2011 rises, and the construction project design for fire protection examination & verification that various places accept and fire control acceptance declare project, answer the requirement of strict implement this notice.To project under construction, as architectural exterior insulation adopts inflammable, combustible matl, NGO competent departments concerned should be submitted to supervise construction unit to remove inflammable, flammable lagging material; To the construction project not yet gone into operation, architectural exterior insulation adopts inflammable, combustible matl, construction unit should be supervised to change design, select non-fire material, again report to a higher authorities for approval.
Therefore, inorganic heat preserving and heat insulation material has had greatly market, and does not also have now the inorganic heat preserving and heat insulation material of the marketization can replace organic heat-insulating lagging material.Current conventional inorganic heat preserving and insulating material can be divided three classes: a class is the constituent material of self heat insulation wall, as foamed concrete, foam geopolymer, gas concrete, diatomite product, heat-insulating calcium silicate product and multicellular glass etc.; One class is the inorganic heat preservation such as rock wool, glass wool fiber; One class is add the thermal insulation mortar of heat preserving aggregate.And the major advantage of inorganic heat preserving and heat insulation material is that fire protection flame retarding, deformation coefficient are little, anti-aging, long service life, eco-environmental prote are good, main drawback is that unit weight is comparatively large, compactness and workability poor, thermal and insulating performance is not as organic insulation material.Also have the inorganic heat preserving and heat insulation material of class large-scale application not yet, the advantages such as be exactly aerogel, it is low that it has thermal conductivity, and unit weight is little, but there is the shortcomings such as the high and bad mechanical strength of preparation cost.
Multicellular glass belongs to the ep-type material that nation-building cause " 12 " is widelyd popularize and applied, there is little, the anti-chemical burn into of density by a series of excellent properties such as the infringement of ant mouse, heat insulating, waterproof and dampproof, fire prevention, sound absorptions, the engineering materials as insulation cold insulation, sound absorption has been widely used in chemical industry, petrochemical industry, light industry, refrigeration, heating installation carries, builds the fields such as environmental protection.But the mechanical strength of multicellular glass is low, easily broken, fracture in processing handling process, and also its anti-folding, ultimate compression strength are all difficult to the requirement meeting building field light-weight high-strength material.Therefore, in order to improve the intensity of multicellular glass, crystallite foam glass enters our visual field.But the preparation technology of crystallite foam glass is very similar with the preparation technology of multicellular glass, but introduce nucleator and heat treated process, add its preparation cost.Produce crystallite foam glass at present, all by powder dress in a mold, mould heats together with powder (blowing temperature is substantially more than 800 DEG C) simultaneously.So except consuming a large amount of whipping agents and the energy, what also have mould loses cost.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of low temperature crystallite foam glass and preparation method thereof, and this crystallite foam glass density is low, and intensity is high, and thermal and insulating performance is good, long service life, and fire resistance is good, and the method is simple to operate, reduces blowing temperature.
A kind of low temperature crystallite foam glass of the present invention, in this crystallite foam glass, the scope of the mol ratio of each main ingredient is: Na
2o (or K
2and SiO O)
2mol ratio be 0.1 ~ 1.0:1, SiO
2with Al
2o
3mol ratio be 1.0 ~ 20:1, B
2o
3with SiO
2mol ratio be 0 ~ 0.2:1.
Network structure (as accompanying drawing 1,2) containing aluminum-oxygen tetrahedron and boron oxygen tetrahedron in glassy phase between the particles of aggregates of described low temperature crystallite foam glass, simultaneously between particles of aggregates and glassy phase or be then be combined (as accompanying drawing 3) with silica silicon key, silica aluminium key or silica boron bond between particles of aggregates and particles of aggregates.
The preparation method of a kind of low temperature crystallite foam glass of the present invention, comprising:
(1) be 0.1≤Na according to mol ratio
2o (K
2o)/SiO
2≤ 1.0,1.0≤SiO
2/ Al
2o
3≤ 20,0≤B
2o
3/ SiO
2≤ 0.2,10≤H
2o/Na
2o≤25 take water glass, reactive aggregate (i.e. Nucleating Agent) and additive, then water glass, reactive aggregate are at room temperature mixed and stir, adding additive afterwards, obtaining full-bodied colloidal sol;
(2) by after the sealing of above-mentioned colloidal sol at 10-80 DEG C aging 1 ~ 7 day, to promote alkali-aggregate reaction; By the colloidal sol after aging 100 ~ 150 DEG C of dryings, obtained water ratio is the solid gel of 10% ~ 50%;
(3) smashed to pieces by above-mentioned solid gel, load in mould, foaming process carries out according to following heat treating regime: intensification foaming stages, with ramp to 250 ~ 500 DEG C of 10 ~ 20 DEG C/min, is incubated 0.5 ~ 10 hour; In the cooling down stage, be down to room temperature with the rate of temperature fall of 2 ~ 30 DEG C/min, obtain low temperature crystallite foam glass.
Water glass described in step (1) is sodium silicate or potash water glass.
Reactive aggregate described in step (1) is one or more in kaolin, metakaolin, volcanic ash, flyash, wilkinite, diatomite, silicon powder, waste glass powder, silicon ash, mineral waste, chainotte.
Additive described in step (1) is one or more in boric acid, borax, silicon sol.
Type of heating in heat treating regime described in step (2) is electrically heated, flame heating or microwave heating.
Low temperature crystallite foam glass of the present invention possesses the cementation of gelling material and the binding structure of organic polymer material, possesses microlitic structure again simultaneously, thus shows high intensity, good endurance quality and good water tolerance etc.The present invention is specifically base with water glass, first under the condition stirred, adds Nucleating Agent and reactive aggregate (as kaolin, metakaolin, volcanic ash etc.), alkali-aggregate reaction is occurred.Add additive (boric acid, borax and silicon sol etc.) afterwards and be stirred to it and dissolve obtained colloidal sol completely.Then at ambient temperature after aging for some time, by solid gel certain for the obtained water ratio of this colloidal sol drying, finally put into mould and high temperature or microwave condition issue brewed must new type low temperature crystallite foam glass.
The present invention take water glass as alkali-activator and whipping agent, and reactive aggregate is Nucleating Agent, adds quantitative additive simultaneously, at low temperatures the new type low temperature crystallite foam glass of the obtained a kind of high strength of foaming.Network structure (as accompanying drawing 1,2) containing aluminum-oxygen tetrahedron and boron oxygen tetrahedron in glassy phase between the particles of aggregates of material, simultaneously between particles of aggregates and glassy phase or be then be combined (as accompanying drawing 3) with silica silicon key, silica aluminium key or silica boron bond between particles of aggregates and particles of aggregates.This structure can give its following characteristics: the network integration key that (1) is formed is covalent linkage, has very high strength; (2) there is not the problem that between crystal and colloid, boundary strength is low; (3) owing to there is not the hydrated product of the easy react with medium, so high erosion-resisting characteristics can be had; (4) near aluminum-oxygen tetrahedron and boron oxygen tetrahedron, there is center of negative charge, can various positively charged ion has been strapped in grid, the water tolerance of the material of raising.Meanwhile, give the performance of its excellence: (1) mechanical property is good, and Main Mechanical index is better than multicellular glass and foamed concrete.(2) impervious good, freeze-thawing resistant circulates, resistance to chemical attack, also can stablize by holding structure in sour environment.
Low temperature crystallite foam glass of the present invention is a kind of cementation possessing gelling material, simultaneously possesses again the novel amorphous of binding structure and crystallite coexists, moisture porous material, and wherein water exists with the form of hydroxyl.Low temperature crystallite foam glass of the present invention is applicable to the heat preserving and insulating material in heat-preserving wall, external-wall exterior insulation layer and other wrapping material.
The present invention not only also reduces blowing temperature from simplifying technique, also maintains crystallite foam glass high strength simultaneously, reduce further thermal conductivity, is expected to replace organic heat-insulating lagging material.
Beneficial effect:
(1) crystallite foam glass of the present invention is inorganic phase entirely, therefore not only has good thermal and insulating performance, and its work-ing life is also longer, can mate with the work-ing life in house, also has excellent fire resistance simultaneously; In addition, also because containing the network structure of aluminum-oxygen tetrahedron and boron oxygen tetrahedron and high void content in material, so the present invention has the feature that density is low and intensity is high equally;
(2) preparation method of the present invention is simple, the temperature preparing crystallite foam glass is reduced greatly, has dropped to less than 500 degree, provide cost savings from more than original 800 degree.
Accompanying drawing explanation
Fig. 1 is the structural representation of the aluminum-oxygen tetrahedron in low temperature crystallite foam glass of the present invention;
Fig. 2 is the structural representation of the boron oxygen tetrahedron in low temperature crystallite foam glass of the present invention;
Fig. 3 is the structural representation of particle in low temperature crystallite foam glass of the present invention;
Fig. 4 is low temperature crystallite foam glass sample photo of the present invention;
Fig. 5 is the electromicroscopic photograph of the surface tissue of low temperature crystallite foam glass of the present invention;
Fig. 6 is the electromicroscopic photograph of the section structure of low temperature crystallite foam glass of the present invention;
Fig. 7 metakaolin is on the impact of low temperature crystallite foam glass ultimate compression strength of the present invention;
Fig. 8 unit weight is on the impact of low temperature crystallite foam glass ultimate compression strength of the present invention;
Fig. 9 is the XRD of low temperature crystallite foam glass of the present invention.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Adopt modulus M=3.0, solid content be 35% Liquid Sodium water glass, boric acid and metakaolin be that raw material carries out serial experiment.Four formulas adopted are respectively A, B, C, D.Their concrete proportioning raw materials are as shown in the table:
The raw material weighing of each formula is good, follow these steps to carry out: first the metakaolin claimed mixed with water glass and stir 1 hour, adding boric acid afterwards and be stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 20% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 300 of 10 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.The low temperature crystallite foam glass obtained according to formula A, B, C, D is carried out correlated performance test, and its result is as shown in the table:
As can be seen from the above table, along with the add-on of metakaolin increases, little on the impact of the rate of weight loss of low temperature crystallite foam glass, coefficient of softening and thermal conductivity.And be fairly obvious on the impact of its ultimate compression strength, trend is as shown in Figure 6.Prepared the sample of the different unit weights of C formula simultaneously, and have studied the impact of unit weight on ultimate compression strength, more high compressive strength is larger for unit weight as shown in Figure 7.
Embodiment 2
According to mol ratio be: Na
2o/SiO
2=0.2, SiO
2/ Al
2o
3=3, B
2o
3/ SiO
2=0.1, H
2o/Na
2o=22 weighs each raw material (sodium silicate, kaolin, silicon ash and borax).First kaolin is calcined three hours obtained metakaolins under 800 degree, then the metakaolin claimed and silicon ash to be mixed with water glass and stir 1 hour, add borax afterwards and be stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 20% at water ratio.Take 250g to load in mould, be warming up to 300 DEG C with speed 10 DEG C/min and be incubated 3h, being finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtaining unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 1.5MPa, thermal conductivity 0.060W/mK, rate of weight loss 0.30%, coefficient of softening 94.8%.
Embodiment 3
According to mol ratio be: Na
2o/SiO
2=0.2, SiO
2/ Al
2o
3=2, B
2o
3/ SiO
2=0.1, H
2o/Na
2o=22 weighs each raw material (sodium silicate, flyash and boric acid).First by claiming flyash to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 20% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 300 of 5 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 1.6Mpa, thermal conductivity 0.060W/mK, rate of weight loss 0.30%, coefficient of softening 94.8%.
Embodiment 4
According to mol ratio be: Na
2o/SiO
2=0.15, SiO
2/ Al
2o
3=6.5, B
2o
3/ SiO
2=0.1, H
2o/Na
2o=25 weighs each raw material (sodium silicate, metakaolin, silicon sol and boric acid).First will claim metakaolin to mix with water glass and to stir 1 hour, add silicon sol afterwards and boric acid is stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 50% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 250 of 5 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 2 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 2.0MPa, thermal conductivity 0.062W/mK, rate of weight loss 0.28%, coefficient of softening 95.8%.
Embodiment 5
According to mol ratio be: K
2o/SiO
2=0.15, SiO
2/ Al
2o
3=6.5, B
2o
3/ SiO
2=0.1, H
2o/K
2o=25 weighs each raw material (potash water glass, chainotte, silicon powder and boric acid).First by claiming silicon powder and chainotte to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 40% at water ratio.Take 250g to load in mould, be incubated 2h with the ramp to 300 of 3 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 1.8MPa, thermal conductivity 0.060W/mK, rate of weight loss 0.26%, coefficient of softening 96.5%.
Embodiment 6
According to mol ratio be: Na
2o/SiO
2=0.3, SiO
2/ Al
2o
3=3.3, B
2o
3/ SiO
2=0.1, H
2o/Na
2each raw material (sodium silicate, volcanic ash and boric acid) is weighed in the scope of O=22.First by claiming volcanic ash to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 10% at water ratio.Take 250g to load in mould, be incubated 5h with the ramp to 400 of 15 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 10 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 1.6MPa, thermal conductivity 0.061W/mK, rate of weight loss 0.30%, coefficient of softening 95.0%.
Embodiment 7
According to mol ratio be: Na
2o/SiO
2=0.2, SiO
2/ Al
2o
3=2, B
2o
3/ SiO
2=0.2, H
2o/Na
2each raw material (sodium silicate, mineral waste and boric acid) is weighed in the scope of O=22.First by claiming mineral waste to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 150 DEG C of dryings, to being 30% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 300 of 18 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 20 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 1.6MPa, thermal conductivity 0.061W/mK, rate of weight loss 0.35%, coefficient of softening 94.8%.
Embodiment 8
According to mol ratio be: Na
2o/SiO
2=0.1, SiO
2/ Al
2o
3=8, B
2o
3/ SiO
2=0.1, H
2o/Na
2each raw material (sodium silicate, metakaolin, silicon powder and boric acid) is weighed in the scope of O=25.First by claiming silicon powder and metakaolin to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 150 DEG C of dryings, to being 20% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 300 of 10 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 2.5MPa, thermal conductivity 0.060W/mK, rate of weight loss 0.29%, coefficient of softening 96.8%.
Embodiment 9
According to mol ratio be: Na
2o/SiO
2=0.1, SiO
2/ Al
2o
3=8, B
2o
3/ SiO
2=0.1, H
2o/Na
2each raw material (sodium silicate, diatomite, silicon powder and boric acid) is weighed in the scope of O=25.First by claiming silicon powder and metakaolin to mix with water glass and to stir 1 hour, adding boric acid afterwards and being stirred to formation colloidal sol, and at room temperature aging 1 day.Then this mixture is after 100 DEG C of dryings, to being 20% at water ratio.Take 250g to load in mould, be incubated 3h with the ramp to 300 of 10 DEG C/min DEG C, be finally down to room temperature with the rate of temperature fall of 5 DEG C/min and namely obtain unit weight for 200kg/m
3low temperature crystallite foam glass.Its ultimate compression strength is 2.5MPa, thermal conductivity 0.060W/mK, rate of weight loss 0.29%, coefficient of softening 96.8%.
Claims (4)
1. a preparation method for low temperature crystallite foam glass, comprising:
(1) according to Na
2o or K
2o and SiO
2mol ratio be 0.1 ~ 1.0:1, SiO
2with Al
2o
3mol ratio be 1.0 ~ 20:1, B
2o
3with SiO
2mol ratio be 0 ~ 0.2:1, H
2o and Na
2the mol ratio of O is that 10 ~ 25:1 takes water glass, reactive aggregate and additive, then water glass, reactive aggregate is at room temperature mixed and stirs, adding additive afterwards, obtain colloidal sol; Wherein, reactive aggregate is Nucleating Agent; Additive is one or more in boric acid, borax, silicon sol;
(2) by the sealing of above-mentioned colloidal sol and aging 1 ~ 7 day, then by the colloidal sol after aging 100 ~ 150 DEG C of dryings, obtained water ratio is the solid gel of 10% ~ 50%;
(3) smashed to pieces by above-mentioned solid gel, load in mould, foaming process carries out according to following heat treating regime: intensification foaming stages, with ramp to 250 ~ 500 DEG C of 10 ~ 20 DEG C/min, and insulation 0.5 ~ 10h; In the cooling down stage, be down to room temperature with the rate of temperature fall of 2 ~ 30 DEG C/min, obtain low temperature crystallite foam glass.
2. the preparation method of a kind of low temperature crystallite foam glass according to claim 1, is characterized in that: the water glass described in step (1) is sodium silicate or potash water glass.
3. the preparation method of a kind of low temperature crystallite foam glass according to claim 1, is characterized in that: the reactive aggregate described in step (1) is one or more in kaolin, metakaolin, volcanic ash, flyash, wilkinite, diatomite, silicon powder, waste glass powder, silicon ash, mineral waste, chainotte.
4. the preparation method of a kind of low temperature crystallite foam glass according to claim 1, is characterized in that: the type of heating in the heat treating regime described in step (2) is electrically heated, flame heating or microwave heating.
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| CN103288353B (en) * | 2013-05-23 | 2015-05-13 | 天津大学 | Borosilicate microcrystalline foam glass with low density and high strength |
| RU2540719C1 (en) * | 2013-10-07 | 2015-02-10 | Общество С Ограниченной Ответственностью "Научно-Производственное Объединение "Диатомит" | Mixture for producing foamed glass |
| CN103755145B (en) * | 2013-12-24 | 2016-04-27 | 宁波荣山新型材料有限公司 | A kind of pressurize expanded method and the equipment thereof of preparing cryogenic foam glass |
| CN104710187B (en) * | 2015-02-15 | 2016-10-05 | 宁夏黑金科技有限公司 | Utilize GUANYINTU and the high intensity crystallite foaming fire preventing and heat insulating board of graphite production and production technology thereof |
| CN105236913B (en) * | 2015-08-20 | 2017-07-11 | 中国科学技术大学先进技术研究院 | A kind of preparation method of fiber reinforcement inorganic heat preservation foam |
| CN107892483A (en) * | 2017-11-11 | 2018-04-10 | 蚌埠承永玻璃制品有限公司 | A kind of insulating foam method for glass preparation |
| CN109399942A (en) * | 2018-11-22 | 2019-03-01 | 宁波荣山新型材料有限公司 | A kind of foam glass Ceramic Composite building heat preservation heat-barrier material and preparation method thereof |
| CN110922159A (en) * | 2019-11-24 | 2020-03-27 | 沈阳理工大学 | Alkali-activated waste brick powder solidified heavy metal ion light heat-insulating material and preparation method thereof |
| CN111362582B (en) * | 2020-04-09 | 2021-01-19 | 浙江大学 | Vacuum foaming low-temperature foam glass material and preparation method and application thereof |
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| CN101445326A (en) * | 2008-12-22 | 2009-06-03 | 天津大学 | High corrosion-resisting foam glass and low-temperature production method thereof |
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| JPS6077145A (en) * | 1983-10-03 | 1985-05-01 | Asahi Chem Ind Co Ltd | Modified inorganic glass foam and production thereof |
| JP2899954B2 (en) * | 1996-06-20 | 1999-06-02 | 英雄 居上 | Porous crystallized glass composition |
| KR100536854B1 (en) * | 2003-10-23 | 2005-12-16 | 한국원자력연구소 | Composition for foam glass and method for preparing foam glass precusor using them |
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