CN102101769A - 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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- CN102101769A CN102101769A CN 200910201253 CN200910201253A CN102101769A CN 102101769 A CN102101769 A CN 102101769A CN 200910201253 CN200910201253 CN 200910201253 CN 200910201253 A CN200910201253 A CN 200910201253A CN 102101769 A CN102101769 A CN 102101769A
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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 the preparation method of a kind of nano silicon micropore thermal insulator and employing sintering temperature and low thereof specifically.This thermal insulator can be applicable to the structure fire of high request occasions such as boats and ships, oceanographic engineering, aerospace and heat insulation.
Background technology
Nano silicon micropore thermal insulator is research both at home and abroad in recent years and use the type material of being paid close attention to.Because this material has low thermal conductivity under hot conditions, in heat insulation demanding occasion very big using value is arranged.Yet the extensive work by domestic and international investigator though 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 just makes the complicated process of preparation of nano-thermal-insulating body, factors such as product molding difficulty, thus be difficult to the reality use of paying.
The forming technique of existing nano silicon micropore thermal insulator mainly contains the three major types type:
The first kind is a 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, be equipped with thermal insulator to apparatus and process conditional request height with this legal system, the product mechanical property is not high, preparation efficiency is low, is difficult to mass and makes.
Second class is a high-temperature sintering process.Promptly adopt 500-900 ℃ sintering temperature to prepare thermal insulator 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 produce the adiabatic bulk of big shape, and it is higher to consume energy.
The 3rd class is to adopt organic adhesive to carry out bonding method.As patent [ZL96196880.X], the thermal insulator of this method preparation 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 at the present material of developing and invent open question still, 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 micropore thermal 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 micropore thermal insulator, it is characterized in that described micropore thermal insulator is made up 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 micropore thermal 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 carried out uniform mixing;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt dull and stereotyped pressing machine that mixture is compressed to required thickness simultaneously; Pressure range is 0.2-2.0MPa;
Step 3, pressurize 5-15 minute are carried out the demoulding then and are 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 promptly became nano silicon micropore thermal insulator goods.
The present invention adopts the method for sintering temperature and low to prepare the high nano silicon micropore thermal 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 at particle contact surface generation fluorine, phosphorus silicic acid class thing, prepare have the intensity height, unit weight is light, thermal conductivity is low nano silicon micropore thermal insulator, beneficial effect is mainly reflected in:
1) can make the moulding of nano silicon micropore thermal insulator 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, the ultimate compression strength that makes thermal insulator is greater than 0.40Mpa.
3) the nano level hole rate height of prepared thermal insulator, 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 height, 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 micropore thermal insulator and has that insulation effect is good, preparation easily, low, the goods of mold temperature can carry out advantages such as cutting processing, can use the high occasion of fire-proof and thermal-insulation technical requirements in industry such as boats and ships, oceanographic engineering, aerospace and other.
Embodiment
The present invention is a kind of nano silicon micropore thermal insulator, it is characterized in that, described micropore thermal insulator is made up 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, 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.Mass ratio M is formed in the mixing of the two
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 is formed 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 micropore thermal 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 carried out uniform mixing;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt dull and stereotyped pressing machine that mixture is compressed to required thickness simultaneously; Pressure range is 0.2-2.0MPa, adopts when specifically implementing and calculates the required design thickness of thermal insulator moulding, adopts dull and stereotyped hydropress compressing mixt to design thickness;
Step 3, pressurize 5-15 minute are carried out the demoulding then, form 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 promptly became nano silicon micropore thermal insulator goods.
Provide embodiments of the invention and concrete preparation method below.Be convenient to comparative illustration, the shape of products of following examples preparation is
180 * 20mm, unit weight 180-220Kg/m
3, be not limited to the present invention.
Embodiment 1:
Each set of dispense ratio of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 60% of an 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 an overall composition quality,
3. inorganic fibre is a basalt fibre, and its consumption is 10% of an 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 an overall composition quality.
The preparation method:
According to each step in the summary of the invention: with each component blending dispersion of the foregoing description 1; Take by weighing the mixture 106.8g that above-mentioned steps obtains after being uniformly dispersed and put into mould, and use dull and stereotyped pressing machine, as the mixture in the mould being depressed into the thickness of 20mm and pressurize 12 minutes with the omnipotent dull and stereotyped hydropress of single-column of 10T, base substrate of demoulding formation then; To put into high temperature oven through the base substrate that above-mentioned steps is pressed at last and react 3 hours down at 200 ℃, naturally cooling is promptly made nano silicon micropore thermal 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 set of dispense ratio of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 85% of an 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 an overall composition quality,
3. inorganic fibre is an aluminum silicate fiber, and its consumption is 3% of an 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 an overall composition quality.
The preparation method:
According to each step in the summary of the invention: with each component blending dispersion of the foregoing description 2, the mixture 91.6g that takes by weighing the above-mentioned steps acquisition after being uniformly dispersed puts into mould, and the mixture in the mould being depressed into the thickness of 20mm and pressurize 5 minutes with the omnipotent dull and stereotyped hydropress of single-column of 10T, the demoulding forms a base substrate then; To put into high temperature oven through the base substrate that is pressed at last and react 2 hours the naturally cooling moulding at 350 ℃ down.
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 set of dispense ratio of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 65% of an 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 an overall composition quality,
3. inorganic fibre is a basalt fibre, and its consumption is 10% of an 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 an 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 the foregoing description 3 is uniformly dispersed and put into mould, and the mixture in the mould being depressed into the thickness of 20mm and pressurize 10 minutes with the omnipotent dull and stereotyped hydropress of single-column of 10T, the demoulding forms a base substrate then; To put into muffle furnace through the base substrate that is pressed at last and react 1 hour the naturally cooling moulding at 450 ℃ down.
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 set of dispense ratio of thermal insulator of the present invention is: (quality percentage composition):
1. nano silicon, its consumption is 55% of an 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 an overall composition quality,
3. inorganic fibre is an aluminum silicate fiber, and its consumption is 3% of an 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 an 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 the mixture in the mould being depressed into the thickness of 20mm and pressurize 15 minutes with the omnipotent dull and stereotyped hydropress of single-column of 10T, the demoulding forms a base substrate then; At last the base substrate that is pressed into is put into muffle furnace and reacted 2.0 hours the naturally cooling moulding at 400 ℃ down.
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 to illustrate technical solution of the present invention, is not limited to the present invention.
Claims (6)
1. nano silicon micropore thermal insulator, it is characterized in that: described micropore thermal insulator is made up 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%.
2. by the described a kind of nano silicon micropore thermal insulator of 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 the described a kind of nano silicon micropore thermal insulator of claim 1, it is characterized in that: described opalizer is the mixture of silicon carbide, titanium dioxide, and mass ratio M is formed in the mixing of the two
Silicon carbide/ M
Titanium dioxideBe 1: 1-3: 1.
4. by the described a kind of nano silicon micropore thermal insulator of claim 1, it is characterized in that: described inorganic fibre is any of basalt fibre or aluminum silicate fiber.
5. by the described a kind of nano silicon micropore thermal insulator of claim 1, it is characterized in that: described reactive behavior agent is the mixture of Sodium Fluoride, aluminium dihydrogen phosphate, and the mixing of the two is formed quality than scope M
Sodium Fluoride/ M
Phosphoric acid dioxy aluminiumBe 1: 10-5: 1.
6. the preparation method of nano silicon micropore thermal 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 carried out uniform mixing;
Step 2, by the mixture that step 1 obtains, be 180-220kg/m by unit weight
3Between weigh and put into mould, adopt dull and stereotyped pressing machine that mixture is compressed to required thickness simultaneously; Pressure range is 0.2-2.0MPa;
Step 3, on dull and stereotyped pressing machine pressurize 5-15 minute are carried out the demoulding then and are 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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| CN102603348A (en) * | 2012-03-14 | 2012-07-25 | 刘相红 | Nano-pore heat-insulation material and manufacturing method thereof |
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| DE10110731A1 (en) * | 2001-02-28 | 2002-10-24 | Ego Elektro Geraetebau Gmbh | Thermal insulation molding |
| GB0505270D0 (en) * | 2005-03-15 | 2005-04-20 | Microtherm Int Ltd | Granular fibre-free microporous thermal insulation material and method |
| CN101219873B (en) * | 2007-01-12 | 2010-05-19 | 上海船舶工艺研究所 | Nano-porous thermal insulating material and method for producing the same |
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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 |
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