CN102101769B - Nano silicon dioxide microporous heat insulator and preparation method thereof - Google Patents
Nano silicon dioxide microporous heat insulator and preparation method thereof Download PDFInfo
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- CN102101769B CN102101769B CN 200910201253 CN200910201253A CN102101769B CN 102101769 B CN102101769 B CN 102101769B CN 200910201253 CN200910201253 CN 200910201253 CN 200910201253 A CN200910201253 A CN 200910201253A CN 102101769 B CN102101769 B CN 102101769B
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Abstract
The invention discloses a nano silicon dioxide microporous heat insulator, which is characterized by consisting of 55 to 85 percent of nano silicon dioxide, 10 to 35 percent of opaquer, 3 to 10 percent of inorganic fibers and 2 to 12 percent of reaction activator. In the invention, the nano silicon dioxide is used as a basic raw material, added with carborundum and titanium dioxide serving as an opaquer, reinforced by basalt fibers or aluminium silicate fibers and subjected to a chemical reaction at a low sintering temperature of 200 to 450 DEG C in the presence of the reaction activator consisting of activator sodium fluoride and aluminium dihydrogen phosphate, so that compounds such as fluosilicate and phosphosilicate are formed on the contact surfaces of the particles of the raw materials to connect the particles of the raw materials into a whole. When the technique disclosed by the invention is used for preparing the nano silicon dioxide microporous heat insulator, the process is simple and the manufacturing is convenient; and the prepared product has high heat insulating performance, and the coefficient of heat conductivity at the average temperature of 500 DEG C is less than or equal to 0.038w/m.k.
Description
Technical field
The invention belongs to the technical field of ceramic, relate to specifically the preparation method of a kind of nano silicon dioxide microporous heat insulator and employing sintering temperature and low thereof.This thermal insulator can be applicable to the structure fire of the high request occasions such as boats and ships, oceanographic engineering, aerospace and heat insulation.
Background technology
Nano silicon dioxide microporous heat insulator is recent domestic research and use the type material of paying close attention to.Because this material has low thermal conductivity under hot conditions, in heat insulation demanding occasion very large using value is arranged.Yet the extensive work by domestic and international investigator although obtained certain achievement and progress in thermal insulation aspect the research of nano material, still exists some technical problems on the moulding process of thermal insulator.This is just so that the complicated process of preparation of nano-thermal-insulating body, the factors such as product molding difficulty, thus be difficult to the reality use of paying.
The forming technique of existing nano silicon dioxide microporous heat insulator mainly contains the three major types type:
The first kind is sol-gel method.As: patent [ZL 95195325.7] is used a large amount of organic solvent extraction moisture in the shaping and drying process, patent [ZL 95108111.X] adopts the supercritical technology moulding, high to the apparatus and process conditional request with the standby thermal insulator of this legal system, the product mechanical property is not high, preparation efficiency is low, is difficult to mass and makes.
Equations of The Second Kind is high-temperature sintering process.Namely adopt 500-900 ℃ sintering temperature to prepare thermal insulator such as patent [US 5556689].This method has improved the physical strength of thermal insulator effectively, but because the restriction of the agglomerating plant under this temperature can't be produced the adiabatic bulk of larger shape, and power consumption is higher.
The 3rd class is to adopt organic adhesive to carry out bonding method.Such as patent [ZL96196880.X], the standby thermal insulator of this legal system under lower use temperature, satisfactory mechanical property.But under greater than 500 ℃ use temperature, the organic adhesive in the thermal insulator all will lose its bond effect, and the structural integrity of thermal insulator goods is destroyed.
Summary of the invention
The objective of the invention is for the present material of developing and invent still open question, overcome above-mentioned technological deficiency, utilize chemical principle, basic demand according to the thermal insulator use, it is low to develop a kind of preparation temperature, and the high nano silicon dioxide microporous heat insulator of use temperature and preparation method thereof.
In order to achieve the above object, technical scheme of the present invention is: a kind of nano silicon dioxide microporous heat insulator, it is characterized in that described microporous heat insulator is comprised of nano silicon, opalizer, inorganic fibre, reactive behavior agent, the mass percent of its each component is:
Nano silicon 55-85%,
Opalizer 10-35%,
Inorganic fibre 3-10%,
Reactive behavior agent 2-12%.
The mass percent sum of each component is 100%.
A kind of preparation method of nano silicon dioxide microporous heat insulator is characterized in that, described preparation method comprises following step:
Step 1, be 55-85% with all powder body materials by nano silicon, opalizer is 10-35%, and the reactive behavior agent is 2-12%, and inorganic fibre is that the mass percent of 3-10% is evenly mixed;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt simultaneously Flat pressure machine that mixture is compressed to required thickness; Pressure range is 0.2-2.0MPa;
Then step 3, pressurize 5-15 minute carried out the demoulding and formed a base substrate;
Step 4, the base substrate of compression moulding in the step 3 is put into baking oven or muffle furnace, between 200-450 ℃ reaction sintering 1-3 hour, the naturally cooling moulding namely became the nano silicon dioxide microporous heat insulator goods.
The present invention adopts the method for sintering temperature and low to prepare the high nano silicon dioxide microporous heat insulator of use temperature, the present invention utilizes fluorine, Phosphorus active compound under the temperature condition between 200-450 ℃, just can make to reach between other material component between the nano silicon and react, also connect in particle contact surface generation fluorine, phosphorus silicic acid class compound, prepare have the intensity height, unit weight is light, thermal conductivity is low nano silicon dioxide microporous heat insulator, beneficial effect is mainly reflected in:
1) can make the nano silicon dioxide microporous heat insulator moulding not being higher than under 450 ℃ the condition, material deformation is little, and can make goods remain on 180Kg/m
3-220Kg/m
3Low unit weight.
2) introducing of response type promoting agent, changed between the nano silicon and and additive between combination, improved the strength of materials, make the ultimate compression strength of thermal insulator greater than 0.40Mpa.
3) the nano level hole rate of prepared thermal insulator is high, and through the sweep electron microscope analysis, its nano level hole rate can reach more than 85%.
4) heat-insulating property is good, detects through the high temperature plane table thermo, and the thermal conductivity of thermal insulator when 500 ℃ of medial temperatures is not more than 0.038w/mk.
5) use temperature is high, and the linear shrinkage ratio under 900 ℃ hot conditions is less than 1%.
A kind of method with sintering temperature and low of the present invention prepares nano silicon dioxide microporous heat insulator and has that insulation effect is good, preparation easily, low, the goods of mold temperature can carry out the advantages such as cutting processing, can use the high occasion of fire-proof and thermal-insulation technical requirements in the industry such as boats and ships, oceanographic engineering, aerospace and other.
Embodiment
The present invention is a kind of nano silicon dioxide microporous heat insulator, it is characterized in that, described microporous heat insulator is comprised of nano silicon, opalizer, inorganic fibre, reactive behavior agent, the mass percent of its each component is: nano silicon 55-85%, opalizer 10-35%, inorganic fibre 3-10%, reactive behavior agent 2-12%.
Wherein said nano silicon is characterized in that particle diameter less than 30nm, and specific surface area is at 200m
2More than/the g, can adopt the commercially available prod, such as Aerosil 200 products such as grade of Degussa company.
Described opalizer is the mixture of silicon carbide powder and titanium dioxide powder, and the powder initial size of silicon carbide and titanium dioxide is less than 250nm.The mixing of the two forms mass ratio M
Carbonization Silicon/ M
Titanium dioxideBe 1: 1-3: 1.
Described inorganic fibre is any in basalt fibre or the aluminum silicate fiber, and the diameter of inorganic fibre is less than 10 μ, and length is 5-20mm;
Described reactive behavior agent is the mixture of Sodium Fluoride, aluminium dihydrogen phosphate, and the mixing of the two forms quality than scope M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 1: 10-5: 1, the diameter of particle of Sodium Fluoride, aluminium dihydrogen phosphate is less than 10 μ.
A kind of preparation method of nano silicon dioxide microporous heat insulator is characterized in that, described preparation method comprises following step:
Step 1, be 55-85% with all powder body materials by nano silicon, opalizer is 10-35%, and the reactive behavior agent is 2-12%, and inorganic fibre is that the mass percent of 3-10% is evenly mixed;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt simultaneously Flat pressure machine that mixture is compressed to required thickness; Pressure range is 0.2-2.0MPa, adopts during implementation and calculates the required design thickness of thermal insulator moulding, adopts the flat plate hydraulic machine compressing mixt to design thickness;
Then step 3, pressurize 5-15 minute carry out the demoulding, forms a base substrate;
Step 4, the base substrate of compression moulding in the step 3 is put into baking oven or muffle furnace, between 200-450 ℃ reaction sintering 1-3 hour, the naturally cooling moulding namely became the nano silicon dioxide microporous heat insulator goods.
The below provides embodiments of the invention and concrete preparation method.Be convenient to comparative illustration, being shaped as of the goods of following examples preparations
180 * 20mm, unit weight 180-220Kg/m
3, be not limited to the present invention.
Embodiment 1:
Each component proportion of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 60% of overall composition quality,
2. opalizer is silicon carbide, titanium dioxide mass ratio M
Silicon carbide/ M
Titanium dioxideBe 3: 1 mixture, its consumption is 25% of overall composition quality,
3. inorganic fibre is basalt fibre, and its consumption is 10% of overall composition quality,
4. the reactive behavior agent is that Sodium Fluoride, aluminium dihydrogen phosphate mixing quality compare M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 1: 10 mixture, its consumption is 5% of overall composition quality.
The preparation method:
According to each step in the summary of the invention: with each component blending dispersion of above-described embodiment 1; Take by weighing the mixture 106.8g that above-mentioned steps obtains after being uniformly dispersed and put into mould, and use Flat pressure machine, as with the omnipotent flat plate hydraulic machine of single-column of 10T the mixture in the mould being depressed into the thickness of 20mm and pressurize 12 minutes, base substrate of demoulding formation then; To put into high temperature oven 200 ℃ of lower reactions 3 hours through the base substrate that above-mentioned steps is pressed at last, naturally cooling is namely made nano silicon dioxide microporous heat insulator.
The effect of the thermal insulator that this example obtains is: unit weight 210Kg/m
3, compressive strength is 0.44Mpa; Thermal conductivity when 500 ℃ of medial temperatures is 0.033w/mk.
Embodiment 2:
Each component proportion of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 85% of overall composition quality,
2. opalizer is silicon carbide, titanium dioxide mass ratio M
Silicon carbide/ M
Titanium dioxideBe 2: 1 mixture, its consumption is 10% of overall composition quality,
3. inorganic fibre is aluminum silicate fiber, and its consumption is 3% of overall composition quality,
4. the reactive behavior agent is that Sodium Fluoride, aluminium dihydrogen phosphate mixing quality compare M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 1: 2 mixture, its consumption is 2% of overall composition quality.
The preparation method:
According to each step in the summary of the invention: with each component blending dispersion of above-described embodiment 2, the mixture 91.6g that takes by weighing the above-mentioned steps acquisition after being uniformly dispersed puts into mould, and with the omnipotent flat plate hydraulic machine of single-column of 10T the mixture in the mould was depressed into the thickness of 20mm and pressurize 5 minutes, then the demoulding forms a base substrate; To put into high temperature oven in 350 ℃ of lower reactions 2 hours, naturally cooling moulding through the base substrate that is pressed at last.
The beneficial effect of this example is: unit weight 180Kg/m
3, compressive strength is 0.40Mpa, the thermal conductivity when 500 ℃ of medial temperatures is 0.038w/mk.
Embodiment 3:
Each component proportion of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 65% of overall composition quality,
2. opalizer is silicon carbide, titanium dioxide mass ratio M
Silicon carbide/ M
Titanium dioxideBe 1: 1 mixture, its consumption is 20% of overall composition quality,
3. inorganic fibre is basalt fibre, and its consumption is 10% of overall composition quality,
4. the reactive behavior agent is that Sodium Fluoride, aluminium dihydrogen phosphate mixing quality compare M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 5: 1 mixture, its consumption is 5% of overall composition quality.
The preparation method:
According to each step in the summary of the invention: take by weighing the mixture 101.7g that above-mentioned steps obtains after each component ratio of above-described embodiment 3 is uniformly dispersed and put into mould, and with the omnipotent flat plate hydraulic machine of single-column of 10T the mixture in the mould was depressed into the thickness of 20mm and pressurize 10 minutes, then the demoulding forms a base substrate; To put into muffle furnace in 450 ℃ of lower reactions 1 hour, naturally cooling moulding through the base substrate that is pressed at last.
The effect of the thermal insulator that this example obtains is: unit weight 200Kg/m
3, compressive strength is 0.42Mpa; Thermal conductivity when 500 ℃ of medial temperatures is 0.035w/mk.
Embodiment 4:
Each component proportion of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 55% of overall composition quality,
2. opalizer is silicon carbide, titanium dioxide mass ratio M
Silicon carbide/ M
Titanium dioxideBe 3: 2 mixture, its consumption is 35% of overall composition quality,
3. inorganic fibre is aluminum silicate fiber, and its consumption is 3% of overall composition quality,
4. the reactive behavior agent is that Sodium Fluoride, aluminium dihydrogen phosphate mixing quality compare M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 1: 1 mixture, its consumption is 7% of overall composition quality.
The preparation method:
According to each step in the summary of the invention: take by weighing the mixture 111.9g that above-mentioned steps obtains after being uniformly dispersed and put into mould, and with the omnipotent flat plate hydraulic machine of single-column of 10T the mixture in the mould was depressed into the thickness of 20mm and pressurize 15 minutes, then the demoulding forms a base substrate; At last the base substrate that is pressed into is put into muffle furnace in 400 ℃ of lower reactions 2.0 hours, naturally cooling moulding.
The effect of the thermal insulator that this example obtains is: unit weight 220Kg/m
3, compressive strength is 0.47Mpa; Thermal conductivity when 500 ℃ of medial temperatures is 0.036w/mk.
The above embodiment only is used for the explanation technical solution of the present invention, is not limited to the present invention.
Claims (4)
1. nano silicon dioxide microporous heat insulator, it is characterized in that: described microporous heat insulator is comprised of nano silicon, opalizer, inorganic fibre, reactive behavior agent, and the mass percent of its each component is:
Nano silicon 55-85%,
Opalizer 10-35%,
Inorganic fibre 3-10%,
Reactive behavior agent 2-12%;
Described opalizer is the mixture of silicon carbide, titanium dioxide, and the mixing of the two forms mass ratio M
Silicon carbide/ M
Titanium dioxideBe 1: 1-3: 1; Described reactive behavior agent is the mixture of Sodium Fluoride, aluminium dihydrogen phosphate, and the mixing of the two forms quality than scope M
Sodium Fluoride/ M
Aluminium dihydrogen phosphateBe 1: 10-5: 1.
2. by a kind of nano silicon dioxide microporous heat insulator claimed in claim 1, it is characterized in that: the particle diameter of described nano silicon is less than 30nm, and specific surface area is at 200m
2More than/the g.
3. by a kind of nano silicon dioxide microporous heat insulator claimed in claim 1, it is characterized in that: described inorganic fibre is any of basalt fibre or aluminum silicate fiber.
4. the preparation method of nano silicon dioxide microporous heat insulator according to claim 1,
It is characterized in that described preparation method comprises following step:
Step 1, be 55-85% with all powder body materials by nano silicon, opalizer is 10-35%, and the reactive behavior agent is 2-12%, and inorganic fibre is that the mass percent of 3-10% is evenly mixed;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt simultaneously Flat pressure machine that mixture is compressed to required thickness; Pressure range is 0.2-2.0MPa;
Then step 3, on Flat pressure machine pressurize 5-15 minute carried out the demoulding and formed a base substrate;
Step 4, the base substrate of compression moulding in the step 3 is put into baking oven or muffle furnace, between 200-450 ℃ reaction sintering 1-3 hour, the naturally cooling moulding.
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| CN102838342B (en) * | 2012-09-27 | 2013-10-30 | 袁江涛 | Dry preparation method of high-temperature resistant nanometer micropore thermal insulation board |
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| CN106495650A (en) * | 2015-09-06 | 2017-03-15 | 襄阳极光新材料科技有限公司 | Super effect heat-insulating heat-preserving material of a kind of mesoporous nano and preparation method thereof |
| CN106116441A (en) * | 2016-06-17 | 2016-11-16 | 无锡英普林纳米科技有限公司 | A kind of micropore heat-barrier material using nanometer embossing to prepare and preparation method |
| CN108314415A (en) * | 2018-04-11 | 2018-07-24 | 贵州创新轻金属工艺装备工程技术研究中心有限公司 | A kind of aluminum electrolysis industry special-purpose nanometer thermal insulation board and preparation method thereof |
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| CN110105043B (en) * | 2019-05-24 | 2021-09-10 | 厦门博赢技术开发有限公司克拉玛依分公司 | Nano ceramic composite heat-insulation steam-injection boiler tube clamp protection device and preparation method thereof |
| CN110256035B (en) * | 2019-06-24 | 2022-06-21 | 广州晖能环保材料有限公司 | Preparation method of high-strength nanometer thermal insulation board and high-strength nanometer thermal insulation board |
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|---|---|---|---|---|
| CN1373104A (en) * | 2001-02-28 | 2002-10-09 | E.G.O.电气设备制造股份有限公司 | Formed heat insulator |
| CN101128404A (en) * | 2005-03-15 | 2008-02-20 | 微热量国际有限公司 | Granular fibre-free microporous thermal insulation material and method |
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