CN102381884B - Method for preparing porous insulation material by microwave heating alkali metal silicate - Google Patents

Method for preparing porous insulation material by microwave heating alkali metal silicate Download PDF

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CN102381884B
CN102381884B CN2011102698688A CN201110269868A CN102381884B CN 102381884 B CN102381884 B CN 102381884B CN 2011102698688 A CN2011102698688 A CN 2011102698688A CN 201110269868 A CN201110269868 A CN 201110269868A CN 102381884 B CN102381884 B CN 102381884B
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heating
microwave
acid
alkali metal
temperature
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CN102381884A (en
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金江
蒋晓勇
张华�
练国峰
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The invention relates to a method for preparing a porous foam insulation material by microwave heating alkali metal silicate, which is characterized in that alkali metal silicate is directly heated by microwave for producing an insulation material with low heat conduction coefficient and the usage temperature of -200 DEG C<=T<=1100 DEG C. The method for preparing porous insulation material by microwave heating alkali metal silicate enables uniform heating from the outside to inside of the raw material, which solves the problems of uneven heating of the raw material, environmental pollution and high dissipating energy caused by heating a heating furnace from outside to inside. The produced material can be used for direct usage after microwave foaming, and enables long-term usage when the temperature is lower than 450 DEG C; the usage temperature of the prepared porous foam insulation material can be raised to 1100 DEG C after being treated by acid. The method of the invention has the advantages of simple production technology, short production period; simultaneously the material has the merits of good heat insulation performance and low density. The inorganic insulation material has excellent fireproof function, and can be used for building insulation as well as external layer insulation for kilns and heating furnaces.

Description

A kind of microwave heating alkalimetal silicate prepares porous thermal insulating material method
Technical field
The invention belongs to and produce the porous thermal insulating field of materials, be specifically related to utilize the aqueous solution of microwave heating alkalimetal silicate to produce porous thermal insulating material method.
Background technology
Energy-saving and emission-reduction are industrial development trend.The lagging material usage quantity is big, requires abundant raw materials and low price.Building thermal insulation material requires material to have fire-proof function preferably; In high temperature low thermal conductivity gas gel lagging material since complex process and costing an arm and a leg use to receive certain limitation.Therefore seek a kind of low price, the inorganic heat insulation material that heat-insulating property is excellent becomes the new trend of lagging material development.The inorganic heat preservation material of construction does not obtain large-scale application; Important reasons is that inorganic building thermal insulation material exists some shortcomings on practical applications; It mainly is the excessive building cost that increases building body of density of some material; The price of lagging material itself is also higher, and thermal conductivity is bigger, not as the good heat insulating of organic insulation material.
The global energy growing tension, the energy dilemma aggravation, the particularly American-European developed country in countries in the world has given to pay attention to fully to the energy-conserving and environment-protective technology.And lagging material is improving energy utilization rate, reduces the energy consumption aspect and has important effect, and therefore exploitation advanced person's heat-insulation and heat-preservation material is significant to energy-saving and emission-reduction.Lagging material refers to that the thermal conductivity of material should be less than 0.12Wm when medial temperature is not more than 623K (350 ℃) -1k -1Foam glass thermal insulation material is widely used in engineering owing to have good fire prevention, thermal insulation, lightweight characteristics.The traditional mode of production method of foam glass mainly is through grinding to form glass powder, the method production that the adding whipping agent foams through heat with the cullet in the productive life.Because the alkalimetal silicate raw material resources are abundant, especially water glass (water glass) low price has been used for some thermal insulation coatings.At present alkalimetal silicate and glass foam production foam glass technology mainly are employed in the stove direct heating foaming or add pore-forming material calcining foaming.Existing technology exists energy utilization rate low, and the poisonous fume quantity discharged is big, and explained hereafter is complicated, and equipment requirements is high, problems such as production cycle length.
The present invention mainly is through microwave direct heating alkalimetal silicate, is not adding the foaming of following short period of time of situation of any whipping agent, prepares the minimum 30kg/m of being of density 3, the minimum cellular insulant that reaches 0.036W/mK of thermal conductivity, can bring up to 1100 ℃ through the s.t. heatproof again.
The present invention utilizes the high efficiency and the homogeneity of microwave heating; Can make the direct from inside to outside even heating of raw material; Solved in the prior art to calcine and caused from outside to inside the heating raw inequality of being heated through process furnace heating and kiln; Pore is inhomogeneous in the material foaming process, and energy utilization rate is low, the problem that environmental pollution is serious.Through s.t. H +Replace Na +, the lagging material use temperature is increased to 1100 ℃, has solved the problem of regular foam glass use temperature low (T≤450 ℃).Microwave heating not only can apply to the production of lagging material, and other aspects also can use in the industry.
Summary of the invention
The purpose of this invention is to provide a kind of aqueous solution, do not adding any whipping agent, add or do not add the method for producing the porous foam lagging material under the situation of filler through the microwave heating alkalimetal silicate.
Another object of the present invention is to make the use temperature of porous foam lagging material be increased to 1100 ℃ through s.t..
The present invention utilizes microwave direct heating alkalimetal silicate to prepare porous foam lagging material method to comprise:
(1) preparation of raw material:
In solid alkali metal silicates, add entry; The preparation alkali metal silicate aqueous solution, the mass percent of alkalimetal silicate is 25-50% in the aqueous solution, perhaps directly uses the industrial alkali metal silicate aqueous solution of alkalimetal silicate as 25-50%; The aqueous solution by 100 milliliters; Add 0~5 gram filler, filler is selected from one or more in aluminum silicate fiber, polycrystalline mullite fibre, mineral wool, ceramic hollow pearl, pearlstone, carbon dust, the flyash, and raw material stirring is even;
(2) moulding: the temperature-resistant material that moulding in the material injecting mould that will stir, mould adopt low microwave to absorb, preferably pottery or glass;
(3) heating: confected materials in the step (2) is directly put into microwave oven together with mould carry out foamable; Microwave oven is generally family expenses or industrial microwave oven, and microwave frequency is 2450 mepses, and be 5-50 minute heat-up time; Preferred 8-35 minute, more preferably 10-25 minute;
(4) demoulding: heated mould is taken out from microwave oven, carry out the demoulding.
When use temperature T≤450 of prepared perforated foams ℃ and there is not the water tolerance requirement, can directly use.
In another embodiment of the invention; If heating 0.4-1 hour can be melted down in step (3) afterwards in the use temperature T of prepared perforated foams≤450 ℃ and when having water tolerance and requiring under 300 ℃; Preferred 0.5-0.8 hour, the water tolerance of its product improved 6 times.
In another embodiment of the present invention; If the use temperature of prepared perforated foams between 450 ℃-1100 ℃, then needs to carry out immersion treatment with acid, soak time is no more than 12 hours; Preferably be no more than 6 hours; The acid intensity that soaks used acid needs greater than silicic acid, and preferred used acid is hydrochloric acid, sulfuric acid or nitric acid, and use temperature can be brought up to 1100 ℃ rapidly.
In above-mentioned embodiment, described alkalimetal silicate is the aqueous solution of alkalimetal silicate, and modulus is 1≤n≤3.7.The density of the porous foam lagging material of preparation is at 30kg/m 3≤ρ≤150kg/m 3
The present invention proposes to use the aqueous solution of microwave heating alkalimetal silicate, does not add any whipping agent, adds or do not add the method that filler prepares porous, expanded lagging material.If using the abundant and low price sodium silicate water glass in source to be raw material, preparing the porous thermal insulating material through microwave heating, the raising environment protection.
The advantage of invention is:
(1) adopt microwave foaming heating means, make material even foaming from inside to outside, pore distribution is more even, microwave heating energy-saving and environmental protection, time cycle weak point, and technology is simple.
(2) foaming need not added any other additive, and the water in the batching has the effect of auxiliary foaming, reduces because of adding environmental pollution that organic whipping agent causes and inflammable problem.
(3) except that special purpose, the material of microwave heating foaming does not need to carry out aftertreatment again, can directly use.
(4) through the H in the acid +Replace Me +(metals ion), silicate generates silicic acid, and heating generates the SiO of holey 2, product can be anti-1100 ℃, improved use temperature fast.
(5) aqueous solution microwave heating of alkalimetal silicate is directly foamed, and foam density is low, and thermal conductivity is low.For example the modulus n of the aqueous solution of water glass (water glass) is 2.2 o'clock, and density is minimum can to reach 30kg/m 3, the product heat-proof quality is better, the thermal conductivity λ≤0.06W/mK of material.
(6) add s.t. after small amount of filler or the moulding in the raw material, heat insulation, mechanical property and water tolerance obtain certain raising.
(7) can be obtained by accompanying drawing, material microstructure is not that aperture is uniformly distributed in the material, and structure is to be piled up with 1~5um gap at the thin slice of 1~2um by thickness to form, and inside configuration has been partitioned into more aperture by thin slice.Material structure has directivity, and cut direction is different, and material heat-proof quality and mechanical property have certain difference.Perpendicular cut the material heat-proof quality and be superior to the crosscut material, 23 ℃ of room temperatures, during fiber add-on 1.35%, the thermal conductivity of material is minimum, and its value is 0.043Wm-1k-1; And the compressive strength of crosscut material is perpendicular 3~4 times of cutting material, and the maximal pressure intensity that contracts reaches 0.64MPa.
When (8) not having treated material use temperature to be lower than 450 ℃, shrinking percentage is about 5%, and structure is more stable; Shrinking percentage has reached 32.88% in the time of use temperature T=500 ℃, and illustrative material is destructurized greater than 450 ℃.
Directly the foam heat-proof quality and the mechanical property of lagging material of aqueous solution preparation of alkalimetal silicate of microwave is better, and technology is simple, and cost of material is cheap, under high temperature kiln insulation, building exterior wall heat preserving and coldcondition, is incubated to have broad application prospects.
Description of drawings
Fig. 1 is that magnification is 300 lagging material SEM figure.
Fig. 2 is that magnification is 3000 lagging material SEM figure.
Embodiment
Embodiment 1:
(1) preparation of raw material: with the modulus is n=2.2, Na 2O massfraction 10.85%, SiO 2The water glass 100ml of massfraction 24.15% is a raw material;
(2) moulding: directly add in the columniform ceramic die above raw material;
(3) heating means: use frequency to be 2450MHz, power is 800W, heats 12 minutes;
(4) demoulding step: take out ceramic die, the demoulding.
Sample rate is ρ=45kg/m 3, thermal conductivity is 0.041W/mK, compressive strength has heat-proof quality preferably at 0.38MPa.
Embodiment 2:
(1) preparation of raw material:
---with modulus n=3.2, Na 2O massfraction 9.3%, SiO 2The water glass 100ml of massfraction 20.8% is a raw material,
---take the aluminum silicate fiber 2g (length is 2~5 millimeters) that machine is sheared, add water glass and stirring fast;
(2) moulding: directly add in the columniform ceramic die raw material of step (1);
(3) heating means: use frequency to be 2450MHz, the microwave heating of power 680W 10 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
Sample rate is ρ=80kg/m 3, temperature is thermal conductivity λ=0.045W/mK in the time of 200 ℃, has heat-proof quality preferably; Ultimate compression strength reaches 0.72MPa; Through 400 ℃ of sintering, linear shrinkage ratio is 1.85 * 10 -6M/ ℃.
Embodiment 3:
(1) preparation of raw material:
Get the 20g anhydrous sodium metasilicate, add water glass 50ml (modulus is n=3.2, and the mass percent of alkalimetal silicate is 30%), opalizer carbon dust 0.38g evenly stirs.
(2) moulding: directly add in the columniform ceramic die raw material of step (1);
(3) heating means: put into microwave oven, frequency is 2450 megahertzes, and power is 800W, heats 7 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
Sample is a grey black, and density is ρ=67.9kg/m 3, thermal conductivity λ=0.055W/mK.
Embodiment 4:
(1) preparation of raw material:
Measure volume 100ml, modulus n=3.2, Na 2O massfraction 9.3%, SiO 2The water glass of massfraction 20.8% is raw material, adds the 3g polycrystalline mullite fibre, stirs.
(2) moulding: directly add in the columniform ceramic die raw material of step (1);
(3) heating means: put into microwave oven, frequency is 2450 megahertzes, and power is 680W, heats 11 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
(5) sample is cut into 4 * 2 * 2cn, with the salt soak of pH=1 12 hours, be soaked in water 1 hour again, dry back use temperature can reach 1100 ℃.
Sample rate is ρ=85kg/m 3, thermal conductivity is 0.039W/mK, has heat-proof quality preferably.Ultimate compression strength P is 0.1MPa; Behind 1100 ℃ of sintering, linear shrinkage ratio is 0.29 * 10 -6M/ ℃ -1
Embodiment 5:
(1) preparation of raw material:
Measure volume 100ml, modulus n=3.2, Na 2O massfraction 9.3%, SiO 2The water glass of massfraction 20.8% is raw material, and the Starso of weighing 50g modulus n=1 adds the 3g polycrystalline mullite fibre, mixing and stirring.
(2) moulding: directly add in the columniform ceramic die raw material of step (1);
(3) heating means: put into microwave oven, frequency is 2450 megahertzes, and power is 800W, heats 15 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
Sample rate is ρ=50kg/m 3, thermal conductivity is 0.049W/mK, has heat-proof quality preferably, foam volume is the twice of not adding Starso.
Embodiment 6:
(1) preparation of raw material:
Measure volume 3000ml, modulus n=3.2, Na 2O massfraction 9.3%, SiO 2The water glass of massfraction 20.8% is raw material.
(2) moulding: directly add in the columniform ceramic die raw material of step (1);
(3) heating means: put into microwave oven, frequency is 2450 megahertzes, and power is 9000W, heats 23 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
Sample rate is ρ=72kg/m 3, thermal conductivity is 0.049W/mK, has heat-proof quality preferably.
Embodiment 7:
(1) preparation of raw material:
Measure volume 6000ml, modulus n=3.2, Na 2O massfraction 9.3%, SiO 2The water glass of massfraction 20.8% is raw material, adds the 30g fiber, stirs.
(2) moulding: directly add rectangle to the raw material of step (1) (in the ceramic die of 800mm * 600mm * 300mm);
(3) heating means: put into microwave oven, frequency is 2450 megahertzes, and power is 9000W, heats 47 minutes;
(4) demoulding step: take out ceramic die, carry out the demoulding.
Sample rate is ρ=87.6kg/m 3, thermal conductivity is 0.051W/mK, has heat-proof quality preferably.

Claims (9)

1. a microwave direct heating alkalimetal silicate prepares porous foam lagging material method, comprising:
(1) preparation of raw material:
In solid alkali metal silicates, add entry and prepare alkali metal silicate aqueous solution; Wherein the mass percent of alkalimetal silicate is 25-50% or directly uses the aqueous solution of alkalimetal silicate mass percent as 25-50% in the aqueous solution; The aqueous solution by 100 milliliters; Add 0~5 gram filler, filler is selected from one or more in aluminum silicate fiber, polycrystalline mullite fibre, mineral wool, ceramic hollow pearl, pearlstone, carbon dust, the flyash, and raw material stirring is even;
(2) moulding: with moulding in the material injecting mould that stirs, the temperature-resistant material that mould adopts low microwave to absorb;
(3) heating: confected materials in the step (2) is directly put into microwave oven together with mould carry out foamable, its microwave oven is family expenses or industrial microwave oven, and the frequency of microwave oven is 2450 mepses, and be 5-50 minute heat-up time.
(4) demoulding: heated mould is taken out from microwave oven, carry out the demoulding, prepared perforated foams can directly use being lower than under 450 ℃ the temperature.
2. method according to claim 1, wherein said alkalimetal silicate are the aqueous solution of sodium silicate solid or sodium silicate, and modulus is 1≤n≤3.7.
3. according to the described method of one of claim 1-2, be 8-35 minute wherein said heat-up time.
4. according to the described method of one of claim 1-3, be 10-25 minute wherein said heat-up time.
5. according to the described method of one of claim 1-4, wherein said mould is pottery or glass material.
6. according to the described method of one of claim 1-5, if the use temperature of prepared perforated foams is lower than 450 ℃ and when having water tolerance and requiring, in the step (3) of aforesaid method afterwards, temperature is melted down heating 0.4-1 hour greater than 250 ℃.
7. according to the described method of one of claim 1-5; If the use temperature of prepared perforated foams is between 450 ℃-1100 ℃; Then carry out immersion treatment with acid, soak time is no more than 12 hours, soaks the acid intensity of the acid intensity of used acid greater than silicic acid.
8. method according to claim 7, wherein soak time is no more than 6 hours, and used acid is hydrochloric acid, sulfuric acid or nitric acid.
9. require each method according to aforesaid right, the density of wherein prepared porous foam lagging material is at 30kg/m 3≤ρ≤150kg/m 3
CN2011102698688A 2011-09-14 2011-09-14 Method for preparing porous insulation material by microwave heating alkali metal silicate Expired - Fee Related CN102381884B (en)

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CN105819817B (en) * 2016-03-18 2018-08-07 武汉理工大学 A kind of preparation method of the blocky fly ash base heat-insulating material of microwave radiation technology foaming
CN105859240B (en) * 2016-05-11 2018-11-23 泰州市梦之谷科技发展有限公司 A kind of acoustic material and preparation method thereof
CN107840631A (en) * 2017-11-14 2018-03-27 广西吉宽太阳能设备有限公司 A kind of preparation method of high temperature resistant porous insulation material
CN113336528B (en) * 2021-07-06 2022-12-09 蚌埠学院 Foamed ceramic material taking quartz sand tailings as raw material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717263A (en) * 2009-11-24 2010-06-02 高申明 Method for preparing forsterite by roasting silicate olivine ore with microwave
CN101955356A (en) * 2010-10-09 2011-01-26 同济大学 Tunable dielectric barium strontium titanate based composite silicate microwave dielectric material and preparation thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717263A (en) * 2009-11-24 2010-06-02 高申明 Method for preparing forsterite by roasting silicate olivine ore with microwave
CN101955356A (en) * 2010-10-09 2011-01-26 同济大学 Tunable dielectric barium strontium titanate based composite silicate microwave dielectric material and preparation thereof

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