CN107663102B - Inorganic light heat-insulating material and method thereof - Google Patents
Inorganic light heat-insulating material and method thereof Download PDFInfo
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- CN107663102B CN107663102B CN201610601209.2A CN201610601209A CN107663102B CN 107663102 B CN107663102 B CN 107663102B CN 201610601209 A CN201610601209 A CN 201610601209A CN 107663102 B CN107663102 B CN 107663102B
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
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Abstract
The invention provides an inorganic light heat-insulating material and a method thereof, wherein the inorganic light heat-insulating material is obtained by low-temperature cryogel solidification molding and sintering of silica sol and hollow glass beads, and the addition amount of the hollow glass beads is 10-25% of the total mass of the silica sol and the hollow glass beads. The invention has simple and high-efficiency process, and does not need to add any organic additive except silica sol and hollow glass beads in the process, thereby having no environmental pollution; the invention adopts a special hollow glass bead treatment process, increases the surface activity of the hollow glass beads, and improves the compatibility and the dispersibility of the hollow glass beads and silica sol.
Description
Technical Field
The invention relates to an inorganic light heat-insulating material and a method thereof, belonging to the technical field of inorganic light materials.
background
At present, the inorganic light heat-insulating material is prepared by adopting a mechanical stirring foaming method more frequently, and the light material prepared by the method generally has the problems of poor stability of preparation process, complex process, poor water resistance of the material, environmental pollution and the like to different degrees by adding a surfactant and mechanically stirring and foaming.
Hollow Glass Beads (HGB) are a novel light inorganic non-metallic material which is developed in recent years and has wide application and excellent performance, and the Hollow Glass Beads (HGB) mainly comprise borosilicate and are Hollow spheres with the particle size of 10-250 mu m and the wall thickness of 1-2 mu m. It has the advantages of light weight, stable chemical performance, good thermal stability, high electrical insulation, and the like. The surface is smooth and hard, the water absorption is not easy, the influence on the viscosity and the fluidity of the matrix is small even if the filling amount is high, and the nano-particles can be used as an additive for preparing a light material with low density, low viscosity, low permeability and strong binding force. The hollow glass beads are added as filling materials, so that the density of the material is reduced, the moisture absorption, rigidity and insulativity of the material are improved, the compressive strength and impact strength of the material are improved, and the hollow glass beads are widely applied to the fields of building materials, plastics, rubber, coatings, navigation, aerospace and the like.
In recent years, hollow glass beads serving as novel inorganic powder filler are mainly used for filling modification of engineering plastics and rubber, so that the hollow glass beads have the advantages of excellent rheological processing, impact resistance and the like. Currently, filling of polyvinyl chloride, polyethylene, polypropylene, polyamide, polycarbonate, silicone resin, and the like is being studied more. For inorganic salt materials, the hollow glass beads are subjected to high-temperature (above 1000 ℃) treatment in preparation, and the hollow glass beads shrink and crack under long-term high-temperature conditions, so that the hollow glass beads are rarely used for modifying the inorganic salt materials. Meanwhile, the hollow glass beads are subjected to surface treatment when being added into a matrix material, and the surfaces of the hollow glass beads are generally modified by adopting chemical reaction modification, surface coating modification, high-energy surface modification, a chemical plating method and the like, so that the compatibility between the hollow glass beads and the matrix material is improved, and the dispersibility of the hollow glass beads is improved; however, in practice, due to the small diameter of the hollow glass beads, the modification effect of the modification methods is not ideal, and the modification technology is complex.
Disclosure of Invention
the invention aims to overcome the defects of the prior art and provide an inorganic light heat-insulating material which has simple and efficient process, no environmental pollution, homogeneity and high strength and a method thereof.
The technical solution of the invention is as follows: an inorganic light heat-insulating material is prepared from silica sol and hollow glass beads through low-temperature freezing, gel solidification, shaping and sintering, wherein the addition amount of the hollow glass beads is 10-25% of the total mass of the silica sol and the hollow glass beads.
The silica sol used in the invention is commercially available, the content of the nano SiO 2 is generally 15-30%, the silica sol is used as a base material, the slurry is solidified at low temperature, the addition amount of the hollow glass beads is 10-25% of the total mass of the silica sol and the hollow glass beads, if the addition amount is too small, the solid content in the mixed slurry consisting of the silica sol and the hollow glass beads is too low, the product can collapse when the frozen gel is dried, and if the addition amount is too large, the hollow glass beads cannot be uniformly dispersed into the silica sol.
the hollow glass beads used in the invention are commercially available, the particle size range of the hollow glass beads is generally 10-100 mu m, and the hollow glass beads are better in dispersion uniformity in silica sol. The hollow glass beads are subjected to pre-sintering treatment, so that the surface activity of the hollow glass beads is increased, the physical and chemical properties of the surfaces of the hollow glass beads are improved, the compatibility with silica sol and the dispersibility in the silica sol are enhanced, the mechanical strength and the comprehensive performance of the material are improved, and the process is simple.
The specific pre-sintering process of the hollow glass beads comprises the following steps: after the room temperature is raised to 400 +/-5 ℃, the temperature is raised from 400 +/-5 ℃ to 600 +/-5 ℃ within 1.5-2 hours, the temperature is kept at 600 +/-5 ℃ for 10-30 minutes, and then the mixture is naturally cooled to the room temperature for later use. The speed of heating to 400 +/-5 ℃ at room temperature can be selected according to the requirements of heating capacity and energy consumption, the heating rate and the treatment time at high temperature are controlled after about 400 ℃, if the heating rate of the hollow glass beads is too high between 400 and 600 ℃, the hollow glass beads shrink greatly and can cause cracking and collapse, and after the subsequent addition of silica sol, the silica sol enters the hollow glass beads, so that the sedimentation of the hollow glass beads is caused, and the dispersion uniformity of the hollow glass beads in the silica sol is influenced; if the speed is too slow, the hollow glass beads are too long at high temperature, and the hollow glass beads are also greatly shrunk to cause cracking and collapse. Therefore, the invention determines the optimal heating rate and high-temperature treatment time, so that the hollow glass microspheres are slowly and uniformly heated.
The heat preservation time of the invention at about 600 ℃ is also limited by the reasons, the time is determined to be 10-30 minutes, if the time is too short, the surface activity of the hollow glass beads is insufficient, and the compatibility with silica sol is reduced; too long time, too long time of hollow glass microsphere under high temperature, also can make hollow glass microsphere shrink greatly, cause the fracture and collapse.
The change in the pre-sintering process range required by the invention has little influence on the surface activity improvement effect of the hollow glass beads, and the change can be ignored in engineering.
A method for preparing inorganic light heat-insulating material is realized by the following steps:
Firstly, pre-burning hollow glass beads,
After the temperature of the hollow glass microspheres is increased to 400 +/-5 ℃ from room temperature, the temperature is increased to 600 +/-5 ℃ from 400 +/-5 ℃ within 1.5-2 hours, and the temperature is kept at 600 +/-5 ℃ for 10-30 minutes;
The second step, preparing mixed slurry,
Taking silica sol as a liquid phase, adding a certain amount of hollow glass beads subjected to the first-step presintering treatment, and uniformly mixing, wherein the adding amount of the hollow glass beads is 10-25% of the total mass of the silica sol and the hollow glass beads;
Thirdly, curing the low-temperature gel,
Injecting the mixed slurry obtained in the second step into a mold, fully curing and molding the mixed slurry at a low temperature, and demolding to obtain a blank;
the invention utilizes low-temperature silica sol to carry out gelatinization to realize rapid curing molding of the green body, and the cured and molded green body has higher strength, is easy to demould and can be directly heated, dried and sintered. The process is simple to operate, the conditions are easy to control, the formed blank is complete in structure after being dried, shrinkage and deformation do not exist, the product yield is high, the production period is short, and the production cost is low.
2The low-temperature gelling process of the silica sol is irreversible, once frozen, a blank body is cured and formed, and cannot be melted or deformed after being heated, the drying process is completed under normal pressure without vacuum condition or strict control of drying temperature, and the low-temperature is less than or equal to-40 ℃, and liquid nitrogen or other freezing forms can be adopted.
The invention realizes the in-situ near-net-size forming of the slurry by low-temperature silica sol gelation, most of the frozen moisture in the blank prepared by the invention can be sublimated and removed in a completely frozen state, and the removal of the frozen moisture is accelerated only by heating. Compared with other drying methods, the method has the advantages that the change of the physical structure and the molecular structure of the blank is extremely small, the organization structure and the appearance form of the blank are well preserved, the blank is almost not shrunk in the forming and drying processes, the internal stress cannot be generated in the blank, and the blank is not easy to crack in the drying and sintering processes.
And fourthly, drying and sintering to obtain the inorganic light heat-insulating material.
The green body can be dried under normal pressure, the drying temperature is not strictly limited, the green body can be dried at normal temperature, the temperature can be optionally selected below 200 ℃ according to needs, the drying time is 2-48 hours, and the green body is selected according to the drying temperature and the drying degree of the green body, so that the green body is finally and completely dried.
Sintering of green bodies is a well-known technique in the art, and the sintering temperature is generally around 800 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention has simple and high-efficiency process, and does not need to add any organic additive except silica sol and hollow glass beads in the process, thereby having no environmental pollution;
(2) The invention adopts a special hollow glass bead treatment process, so that the surface activity of the hollow glass beads is increased, and the compatibility and the dispersibility of the hollow glass beads and silica sol are improved;
(3) The inorganic composite material obtained by the invention has the advantages of light weight, good mechanical property, good heat insulation and sound insulation properties and the like, is particularly suitable for preparing products with strict requirements on strength and material density, and has wide application prospect in the aspects of heat insulation;
(4) The density of the inorganic light material can be controlled by adjusting the addition amount of the hollow glass beads;
(5) The invention not only has abundant cellular structures, but also improves the compression resistance and the heat insulation effect of the material while reducing the moisture absorption of the material due to the special closed cell structure of the micro-beads.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention is described in detail below with reference to the attached drawings and specific examples.
As shown in figure 1, silica sol is used as a liquid phase, hollow glass beads are added into the silica sol, the silica sol is uniformly dispersed by mechanical stirring, and then the inorganic light heat-insulating material is obtained by injection molding, freeze-solidification molding, drying and sintering.
example 1
1. Pre-burning hollow glass bead at 400 deg.c for 2 hr, heating to 600 deg.c for 1.5 hr, and maintaining at 600 deg.c for 10 min.
2. And adding the hollow glass beads subjected to pre-sintering treatment into silica sol with the solid content of 25%, and uniformly dispersing to obtain mixed slurry, wherein the adding amount of the hollow glass beads is 25% of the total mass of the slurry.
3. mechanically stirring the mixed slurry, injecting the mixture into a mold, freezing and solidifying the mixture in liquid nitrogen, drying the mixture, and sintering the dried mixture at 800 ℃ to obtain the inorganic light heat-insulating material.
the inorganic light heat-insulating material obtained in the embodiment has the volume density of 0.2g/cm 3, the compressive strength of 1.6MPa and the thermal conductivity of 0.08W/m.K.
example 2
1. pre-burning hollow glass bead at 400 deg.c for 2 hr, heating to 600 deg.c for 1.5 hr, and maintaining at 600 deg.c for 10 min.
2. And adding the hollow glass beads subjected to pre-sintering treatment into silica sol with the solid content of 25%, and uniformly dispersing to obtain mixed slurry, wherein the adding amount of the hollow glass beads is 10% of the total mass of the slurry.
3. Mechanically stirring the mixed slurry, injecting into a mold, freezing and solidifying in liquid nitrogen, and sintering at 800 ℃ to obtain the inorganic light heat-insulating material.
the inorganic light heat-insulating material obtained in the embodiment has the volume density of 0.15g/cm 3, the compressive strength of 0.6MPa and the thermal conductivity of 0.04W/m.K.
The invention has not been described in detail and is in part known to those of skill in the art.
Claims (3)
1. A method for preparing inorganic light heat-insulating material is characterized by comprising the following steps:
firstly, pre-burning hollow glass beads,
after the temperature of the hollow glass microspheres is increased to 400 +/-5 ℃ from the room temperature, the temperature is increased to 600 +/-5 ℃ from 400 +/-5 ℃ within 1.5-2 hours, the temperature is kept at 600 +/-5 ℃ for 10-30 minutes, and then the hollow glass microspheres are naturally cooled to the room temperature;
the second step, preparing mixed slurry,
taking silica sol as a liquid phase, adding a certain amount of hollow glass beads subjected to the first-step presintering treatment, and uniformly mixing, wherein the adding amount of the hollow glass beads is 10-25% of the total mass of the silica sol and the hollow glass beads;
Thirdly, freezing the mixed slurry at low temperature to solidify and form gel;
And fourthly, drying and sintering to obtain the inorganic light heat-insulating material.
2. The method for preparing inorganic light-weight thermal insulation material according to claim 1, wherein: the temperature of the low-temperature frozen gel in the third step is less than or equal to-40 ℃.
3. An inorganic light heat-insulating material obtained by the preparation method of claim 1.
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| CN201610601209.2A CN107663102B (en) | 2016-07-27 | 2016-07-27 | Inorganic light heat-insulating material and method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005162551A (en) * | 2003-12-04 | 2005-06-23 | Sanyo Chem Ind Ltd | Grout material composition |
| CN103601358A (en) * | 2013-11-20 | 2014-02-26 | 天津大学 | Preparation method of silicon dioxide-diboron trioxide low-melting-point glass combined hollow glass bead heat-insulating material |
| CN104108938A (en) * | 2014-07-04 | 2014-10-22 | 航天特种材料及工艺技术研究所 | Preparation method for Sialon ceramic |
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- 2016-07-27 CN CN201610601209.2A patent/CN107663102B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005162551A (en) * | 2003-12-04 | 2005-06-23 | Sanyo Chem Ind Ltd | Grout material composition |
| CN103601358A (en) * | 2013-11-20 | 2014-02-26 | 天津大学 | Preparation method of silicon dioxide-diboron trioxide low-melting-point glass combined hollow glass bead heat-insulating material |
| CN104108938A (en) * | 2014-07-04 | 2014-10-22 | 航天特种材料及工艺技术研究所 | Preparation method for Sialon ceramic |
Non-Patent Citations (1)
| Title |
|---|
| "空心玻璃微珠轻质高强材料的制备与性能研究";申娜娜;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20150515(第05期);B015-158 * |
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