WO2013077477A1 - Procédé de préparation d'un verre mousse à partir de déchets de verre et procédé de prédiction de la plage de moussage de verre à l'aide d'un dilatomètre - Google Patents

Procédé de préparation d'un verre mousse à partir de déchets de verre et procédé de prédiction de la plage de moussage de verre à l'aide d'un dilatomètre Download PDF

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WO2013077477A1
WO2013077477A1 PCT/KR2011/008918 KR2011008918W WO2013077477A1 WO 2013077477 A1 WO2013077477 A1 WO 2013077477A1 KR 2011008918 W KR2011008918 W KR 2011008918W WO 2013077477 A1 WO2013077477 A1 WO 2013077477A1
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Prior art keywords
glass
temperature
foaming
waste glass
waste
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PCT/KR2011/008918
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English (en)
Korean (ko)
Inventor
박상엽
정준기
방희곤
김성진
Original Assignee
강릉원주대학교 산학협력단
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Priority to PCT/KR2011/008918 priority Critical patent/WO2013077477A1/fr
Priority to CN201180076280.9A priority patent/CN104066692B/zh
Priority to KR1020147010824A priority patent/KR101587568B1/ko
Publication of WO2013077477A1 publication Critical patent/WO2013077477A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/08—Other methods of shaping glass by foaming
    • 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
    • C03C1/002—Use of waste materials, e.g. slags
    • 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
    • C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
    • C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating

Definitions

  • the present invention relates to a foamed glass manufacturing method and a foaming section prediction method, specifically, foamed to manufacture the foamed glass through the grinding and heat treatment process without the addition of foaming agent (or foaming agent) from waste glass as a raw material It relates to a method for predicting the foam section of the glass by using the glass manufacturing method and expansion coefficient measuring equipment.
  • Foamed glass is lightweight and shows excellent performance in flame protection, heat insulation, heat resistance, sound absorption, etc., and is used when industrial waterproof, heat resistance, and durability are required. Especially, it is used as a good thermal insulation material and sound absorbing material in structures or buildings.
  • foam glass was already proposed in the late 1930s.
  • a special composition of glass is mixed with a reducing agent, such as carbon, and a foaming agent containing an oxide, sulfate or other type of oxidizing component, pulverized, and then pulverized. It is fired until softened or melted.
  • an oxidation-reduction reaction occurs between carbon and sulfur oxides (or oxidants or oxides of glass), resulting in molten glass containing SO 2 , CO 2 , N 2 , H 2 S or other gases. It forms low-density, thermally conductive and radiation resistant materials and forms glass gases. As a result, for best results, the structure of the glass has a closed pore free from water, water vapor, or other liquids and gases.
  • the glass thus prepared is pulverized and mixed well by adding carbon, which is a foaming aid that reacts with other ingredients to produce a gas that acts as a direct blowing agent, and then mixes the mixed raw glass powder for producing foamed glass in a predetermined container.
  • carbon which is a foaming aid that reacts with other ingredients to produce a gas that acts as a direct blowing agent
  • the present invention is directed to solving this problem of the prior art, which utilizes waste glass to provide an efficient function with uniform pore distribution without the need for melting, hydrolysis or any other pre-processing of the glass to make a special composition. It is an object to provide a process for producing colorless or colored foamed glass without foaming agents.
  • Another object of the present invention is to provide a method for accurately predicting a foam section of glass according to various measurement parameters such as temperature section, temperature increase rate, temperature holding time and cooling rate using an expansion coefficient measuring device.
  • a foamed glass manufacturing method is provided.
  • At least one selected from the group consisting of water, ethyl alcohol, methyl alcohol, and acetone may be used as the solvent of the wet grinding process.
  • the method may further include dry grinding the sodium-silicate or boroalumino-silicate composition waste glass before the grinding by the wet grinding process.
  • the size of the waste glass powder may be in the range of 1 to 10 ⁇ m.
  • the waste glass powder may be a metal oxide added as a colorant, and the metal oxide may be any one or more of cobalt oxide (Co 3 O 4 ) or manganese oxide (MnO 3 ).
  • the metal oxide may be added to the waste glass powder prior to the firing and foaming step or may be added before the grinding step by the wet grinding process.
  • a method for predicting the foaming section of the glass to predict the foaming section of the unfoamed precursor using the shape change curve according to the temperature of the unfoamed precursor measured by the expansion coefficient measuring equipment is provided.
  • the shape change curve according to the temperature is charged with the unfoamed precursor in the expansion coefficient measuring equipment; And measuring the change in length or volume of the unfoamed precursor while raising the unfoamed precursor to a temperature above the foam start temperature of the unfoamed precursor.
  • the shape change curve can be obtained under the condition that the vertical load or the pushing force is 200 cN or less.
  • the shape change curve may be obtained by changing any one or more of a measurement temperature section, a temperature increase rate, a cooling rate, or a temperature holding time.
  • the measurement temperature range is from room temperature to 1400 °C
  • the temperature increase rate is 0.1 ⁇ 50 °C / min
  • the cooling rate is 0.1 ⁇ 50 °C / min
  • the holding time can be changed in the range of 24 hours or less. .
  • the unfoamed precursor may be in the form of a powder or bulk having a certain form.
  • the process is simplified to produce a foamed glass with excellent aesthetic characteristics with a uniform pore structure while easy process control. It can be used in various architectural and environmental articles.
  • the present invention it is possible to accurately predict the glass foam section having various variables by analysis through the expansion coefficient measuring equipment, which helps to control the process and optimize the production process. It can be usefully used for making glass.
  • FIG. 1 is a flow chart showing a foamed glass manufacturing process using waste glass according to the present invention.
  • Example 3 is a result of observing the appearance of the foamed glass prepared according to Example 1 of the present invention.
  • Figure 5 shows the shape change curve obtained by using the expansion coefficient measuring equipment according to an embodiment of the present invention.
  • Figure 6 shows the shape change curve using the expansion coefficient measuring equipment according to embodiments 9 to 12 of the present invention.
  • FIG. 8 is a result of observing the microstructure image of the foam shape before and after the boundary of the foaming point temperature shown in FIG. 7 with an electron microscope.
  • 9A and 9B are cross-sectional views of horizontal and vertical expansion coefficient measuring equipment according to one embodiment used in the method for predicting a foam section of glass of the present invention, respectively.
  • the present invention is characterized by producing foamed glass by directly foaming the waste glass without undergoing other special pretreatment process for the production of the foamed glass using waste glass, which is generally produced in life or industry.
  • Figure 1 shows a flow chart showing step by step the manufacturing method of foamed glass according to an embodiment of the present invention.
  • a method of manufacturing the foamed glass according to the embodiment of the present invention will be described with reference to FIG. 1.
  • sodium-silicate or boroalumino-silicate composition waste glass is prepared as a foamed glass raw material (S1). This is because when the sodium-silicate or boroalumino-silicate composition waste glass is used as a raw material of the foamed glass, the foamed glass can be manufactured without the addition of a foaming agent.
  • the prepared waste glass is ground to prepare a raw material powder for foaming (S2).
  • the prepared waste glass is pulverized by a wet grinding process using a grinding device such as a disk mill, a ball mill.
  • a grinding device such as a disk mill, a ball mill.
  • at least one solvent selected from the group consisting of water, ethyl alcohol, methyl alcohol and acetone may be used.
  • the grinding of the waste glass may proceed through a plurality of steps for efficient grinding.
  • the waste glass may be first coarsely pulverized by a dry method and then secondly pulverized into finer powders by a wet pulverization process.
  • the waste glass powder is immersed in the molding mold without adding a foaming agent, and is manufactured into a molded body by uniaxial and isotropic pressure (S3).
  • This molded body is made of foamed glass through a firing and foaming step (S4) at 600 to 1000 °C (S5).
  • Equation 1 when M in Equation 1 is Na such as a raw material glass having a specific composition, for example sodium-silicate, when water is added, H + ions in water and Na + ions in the glass are hydrolyzed. Are exchanged with each other to form an NaOH alkaline solution (1 Step). Next, OH - ions of the NaOH alkaline solution penetrate the glass and destroy the SiO 2 grazing structure (2Step). Subsequently, during the plastic foaming process, the hydrolysis resulted in the decomposition of the glassy water or OH - component contained in the glass to form bubbles in the softened or molten glass particles, and thus trapped inside the glass particles. As a result, bubbles are formed in the glass to form foamed glass.
  • Na such as a raw material glass having a specific composition
  • sodium-silicate when water is added, H + ions in water and Na + ions in the glass are hydrolyzed. Are exchanged with each other to form an NaOH alkaline solution (1 Step).
  • Foamed glass produced by the manufacturing process according to an embodiment of the present invention has a uniform fine pore structure and may have excellent mechanical properties and excellent aesthetics.
  • the physical properties of the foamed glass manufactured by the above method may exhibit a density value of 287 kg / m 3, porosity of 88%, compressive strength of 1.4 MPa, and thermal conductivity of 0.070 kcal / mh ° C. at 25 ° C. .
  • Colored foam glass can be realized by adding a metal oxide to the waste glass powder as a colorant.
  • the metal oxide used as the colorant may be, for example, cobalt oxide (Co 3 O 4 ) or manganese oxide (MnO 3 ).
  • Co 3 O 4 cobalt oxide
  • MnO 3 manganese oxide
  • Metal oxides which are colorants, may be added to the process of grinding the waste glass.
  • the waste glass powder may be prepared by adding the metal oxide to the waste glass powder prepared by primary coarse grinding of the prepared waste glass by dry grinding, and then performing the second fine grinding by the wet grinding process.
  • the metal oxide may be added to the powder completed until the second fine grinding, and then the subsequent process may be performed.
  • the metal oxide is added before the firing and foaming process, such as adding a metal oxide before crushing the prepared waste glass and proceeding the crushing process, or preparing a final waste glass powder by pulverizing the waste glass and then adding a metal oxide before molding. If it does, it can be any way.
  • the unfoamed precursor refers to a glass that is in a state in which foaming has not yet occurred or in a state in which foaming may occur as it is heated.
  • the unfoamed precursor may be a glass powder or a bulk form (including a molded body formed by pressing the glass powder) having a predetermined shape.
  • both the macroscopic and the microscopic viewpoints are measured by measuring the change in length or volume of the molded product generated by foaming under various conditions using an expansion coefficient measuring device without using such a high temperature microscope. It is possible to predict the foam generation zone and behavior of the glass to be satisfied.
  • the method for predicting the foam section of the glass of the present invention has a technical feature of observing the thermal behavior of the glass by using the curve for shrinkage or expansion through the coefficient of expansion coefficient measuring equipment more accurate foaming in the production of foam glass Enable temperature range setting.
  • Shrinkage and expansion behavior of the glass can be calculated through the following equations 2 and 3, it is possible to derive the change in the length or volume of the glass according to the temperature change based on the equations 2 and 3.
  • ⁇ is called coefficient of liner expansion and means the ratio of length change to temperature change.
  • the coefficient of volume expansion ⁇ is defined as the ratio of the small change in volume with temperature change under constant pressure.
  • the thermal analysis technique for measuring the change in length ( ⁇ L) as a function of temperature and time under a constant load on the sample is based on the TMA method and It can be divided into dilatometry.
  • TMA is to measure the length change according to temperature and function under a constant load
  • dilato method is to measure the length change according to temperature and function under almost no load.
  • ASTM standard and the actual measurement it is common to measure tens of cN in TMA, and the dilato method also applies several tens of cN, so the distinction between the two measurement methods is not significant.
  • a dilatometer uses a displacement measuring sensor called a linear variable differential transformer (LVDT) to measure a change in length, and is composed of a furnace for controlling temperature and a holder for fixing a sample.
  • LVDT linear variable differential transformer
  • the expansion coefficient measuring device may be divided into a horizontal type as shown in FIG. 9A and a vertical type as shown in FIG. 9B.
  • the horizontal type loads the specimen holder 90a containing the specimen 91a horizontally into the heating furnace 92a, while the vertical type loads the specimen holder 90b containing the specimen 91b vertically into the heating furnace 92b.
  • Both horizontal and vertical may be equipped with thermocouples 94a and 94b for measuring the temperature of the specimens 91a and 91b.
  • the specimens 91a and 91b may be subjected to a predetermined load through pushrods 93a and 93b.
  • the horizontal expansion coefficient measuring equipment can be measured under the force of 200cN or less on the push rod 93a
  • the vertical expansion coefficient measuring equipment can be measured under the vertical load of 200cN by the push rod 93b. Can be measured at.
  • the vertical expansion coefficient measuring equipment it is also possible to apply by measuring only the vertical load corresponding to the self load of the push rod (93b).
  • Complementary measurement is possible through the measurement under the pushing force condition using the horizontal expansion coefficient measuring device and under the vertical load condition using the vertical expansion coefficient measuring device, which has the advantage of setting the optimum temperature condition for forming the foam glass. .
  • This expansion coefficient measuring device can be used to grasp the contraction and expansion behavior of the unfoamed precursors in real time to the process of conversion to foamed glass, and furthermore, to change the temperature rise rate, the holding time and cooling rate change in a certain temperature section.
  • the foaming behavior according to the present invention can be observed and analyzed from a macroscopic and microscopic perspective.
  • the temperature range of the temperature range from room temperature to 1400 ° C., the temperature increase rate from 0.1 ° C. to 50 ° C. per minute, the temperature holding time from 0 to 24 hours, and the cooling rate from 0.1 ° C. to 20 ° C. per minute Foaming behavior due to shrinkage and expansion can be observed in real time.
  • FIG. 5 shows a curve showing an example of shrinkage and expansion behavior of sodium-silicate glass obtained using a horizontal expansion coefficient measuring device (referred to as a shape change curve).
  • the shape change curve is charged with a molded product of sodium-silicate glass powder into the expansion coefficient measuring equipment, and heated at a temperature increase rate of 5 ° C./minute from room temperature to 700 ° C. under a load of 25 cN and maintained at 700 ° C. for 120 minutes. It is the result of measuring the change in shape such as the length or volume of the glass generated during the cooling time to room temperature at the cooling rate of °C / min.
  • the x-axis represents time
  • the y-axis on the left side represents linear shrinkage ( ⁇ L / L,%)
  • the y-axis on the right side represents temperature.
  • 5 shows a change in temperature with time
  • Section 3 represents the volume change of the glass according to the decrease of the temperature, it is possible to observe in real time the shrinkage of the foam glass and the occurrence of cracks during cooling due to the decrease in the cooling temperature.
  • the foaming section of the glass may be measured in real time by measuring a change in shape such as a length change or a volume change in the foaming process of the glass. Therefore, when the foaming section measurement method is utilized, the foaming characteristics according to various foaming conditions, for example, temperature conditions, temperature raising conditions, and holding time conditions, can be known. Optimization of various conditions suitable for the production of glass can be carried out.
  • Sodium-silicate composition waste glass was first ground using a disk mill. Grinding conditions were pulverized by recycling method up to three times. The primary milled powder (average 120 ⁇ m) was subjected to secondary wet milling (average 2 ⁇ m) for 1-72 hours at a speed of 100 ⁇ 400rpm using distilled water as a solvent using planetary mill.
  • the secondary pulverized powder was dried at 60 ° C. for 24 hours using an oven.
  • the dried powder was sieved using a 200 mesh sieve.
  • the powder, which was sieved as a non-foamed precursor was put into a molding mold and molded by a pressure press method to prepare a non-foamed precursor.
  • the foamed glass was manufactured by firing and foaming for 2 hours (Example) 1 to 4).
  • Table 1 shows the specific conditions of Examples 1-4.
  • Example 1 Example 2
  • Example 3 Example 4 Temperature rise rate (°C / min) One 5 10 20 Firing temperature 700 °C 700 °C 700 °C 700 °C Firing time (hours) 2 2 2 2 2
  • FIGS. 2A to 2D show the results of observing the microstructure of the foamed glass prepared according to Examples 1 to 4 of the present invention, respectively, with an electron microscope.
  • Figure 2a to 2d it can be seen that the produced foam glass is uniformly formed pores are distributed, the average size of the pores increases with increasing the temperature increase rate.
  • Figure 3 shows the result of observing the appearance of the foam glass of Example 2.
  • Examples 5 to 8 relate to color foamed glass in which a predetermined color is colored on the foamed glass of Examples 1 to 4.
  • the sodium-silicate composition waste glass was first pulverized using a disk mill. 1 or 2% by weight of cobalt oxide (Co 3 O 4 ) or manganese oxide (MnO 3 ) was added to the first pulverized powder (average 120 ⁇ m) as a colorant, followed by distilled water as a solvent. Secondary wet grinding (average 2 ⁇ m) was performed for a time.
  • the secondary milled powder was dried at 60 ° C. for 24 hours using an oven.
  • the dried powder was sieved using a 200 mesh sieve.
  • the sieved powder was put in a molding mold and molded by a pressure press method to prepare an unfoamed precursor.
  • the non-foamed precursor was used to prepare a foamed glass having various colors through a firing and foaming process at 700 ° C. for 2 hours at a temperature increase rate of 5 ° C. per minute.
  • Table 2 shows the specific conditions of Examples 5 to 8 and the color of the foamed glass.
  • Example 5 Example 6
  • Example 7 Ingredient Co 3 O 4 Co 3 O 4 MnO 3 MnO 3 Composition (% by weight) One 2 One 2 Firing temperature 700 °C 700 °C 700 °C 700 °C Firing time (hours) 2 2 2 2 color grey Dark blue Ultramarine Blue Mauve
  • Figure 4 shows the results of observing the color of the foamed glass prepared according to Examples 5 to 8 of the present invention in the order of the upper left, upper right, lower left and lower right, respectively.
  • Manganese Oxide (MnO 3 ) was added 1% by weight, the color was dark blue, and the density was 202 kg / m 3, but the addition of 2% by weight was light purple and the density was 306 kg / m 3.
  • the foamed glass having the desired color and density can be produced by appropriately adjusting the amount of the coloring agent in consideration of both the color and the density of the foamed glass.
  • An unfoamed precursor was prepared by forming a sieve of powder and molding using a molding mold to enable foam glass section prediction using a sodium-silicate composition glass.
  • the prepared unfoamed precursor was charged into an expansion coefficient measuring instrument and a 25cN load was applied to observe the behavior of the foamed glass in real time while changing the temperature increase rate to 1, 5, 10, 20 ° C / min as shown in Table 3. (Examples 9-12).
  • Example 10 Example 11
  • Example 12 Temperature rise rate (°C / min) One 5 10
  • Load change (cN) 25 25 25 25
  • FIG. 6 shows a shape change curve showing the shrinkage and expansion behavior of the unfoamed precursor when the temperature increase rate is changed to 1, 5, 10, and 20 ° C. per minute.
  • the unfoamed precursor contracts linearly but the volume expands linearly again due to bubbles formed by foaming at a predetermined temperature, that is, the foaming start temperature.
  • the foaming start temperature of the unfoamed precursor increases as the temperature increase rate increases.
  • FIG. 7 shows a shape change curve according to temperature when the temperature increase rate is 5 ° C./minute, and shows that the foaming start temperature is 693 ° C.
  • 8A, 8B and 8C show the microstructure of foamed glass at 673 ° C, 693 ° C and 713 ° C shown in FIG.
  • Porosity is not observed at a temperature lower than the foaming start temperature (FIG. 8A), but pores are observed at the foaming start temperature (FIG. 8B) and relatively coarse due to active foaming at a temperature higher than the foaming start temperature (FIG. 8C). It can be seen that the generated pores are observed.
  • the foamed glass having optimum physical properties can be produced by controlling the foaming conditions by using the foaming behavior curve in the foamed glass production.

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Abstract

Conformément à un aspect de la présente invention, il est proposé un procédé de préparation d'un verre mousse à partir de déchets de verre comprenant les étapes de : mettre sous pression une poudre de déchets de verre comprenant du silicate de sodium ou du boroaluminosilicate de sodium sans ajouter un agent de moussage dans un moule pour préparer un produit moulé; et cuire et faire mousser le produit moulé à 600-1000°C, suivant lequel un procédé de préparation de la poudre de déchets de verre comprend l'étape de pulvérisation des déchets de verre comprenant du silicate de sodium ou du boroaluminosilicate de sodium par pulvérisation par voie humide.
PCT/KR2011/008918 2011-11-22 2011-11-22 Procédé de préparation d'un verre mousse à partir de déchets de verre et procédé de prédiction de la plage de moussage de verre à l'aide d'un dilatomètre WO2013077477A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
PCT/KR2011/008918 WO2013077477A1 (fr) 2011-11-22 2011-11-22 Procédé de préparation d'un verre mousse à partir de déchets de verre et procédé de prédiction de la plage de moussage de verre à l'aide d'un dilatomètre
CN201180076280.9A CN104066692B (zh) 2011-11-22 2011-11-22 使用废玻璃制造泡沫玻璃的方法以及使用膨胀计预测玻璃的发泡范围的方法
KR1020147010824A KR101587568B1 (ko) 2011-11-22 2011-11-22 폐유리를 이용한 발포유리 제조방법

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CN107417099A (zh) * 2016-05-24 2017-12-01 胡斯友 一种高性能环保轻石的制备方法
CN110668700B (zh) * 2019-11-12 2021-09-03 上海超高环保科技股份有限公司 利用废玻璃的耐高温烧结过滤板制造方法
CN114436536A (zh) * 2020-11-02 2022-05-06 毛闻达 一种锂辉石微晶泡沫玻璃及其制备方法

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