CN103524111B - Porous composite aerogel material as well as preparation method and application thereof - Google Patents
Porous composite aerogel material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a porous composite aerogel material. The method comprises the following steps of: prefabricating reinforcement, placing the reinforcement in a reaction container, sealing and vacuumizing, sucking prefabricated sodium silicate liquor until the reinforcement is submerged; pumping an acidic gas in, heating up, then standing to form a wet gel reinforcement composite; pumping in surfactant aqueous liquor for immersion reaction, rotating the wet gel reinforcement composite so that liquid liquor in the composite is thrown out; stopping rotation, pumping in mixed liquor of an organic solvent and the surfactant, discharging overflowed liquor after reaction; heating up, evaporating the organic solvent, carrying out vacuum treatment, and releasing pressure to obtain the porous composite aerogel material. The preparation method related in the invention can be used for obtaining the porous composite aerogel material which has the advantages of low heat conduction efficiency, good hydrophobic performance and high hydrophobic performance and low cost and is simple to operate.
Description
Technical field
The present invention relates to Material Field, particularly relate to a kind of porous aerogel composite and preparation method thereof and application.
Background technology
The aerogel production technique of present appearance, majority is discontinuous operation, or implementation step is carried out in the multiple link in multiple region, the aerogel of manufacture is also compare narrow sense " aerogel ", the middle external force by multiple link affects, and some wet gel skeleton caves in, then carries out drying, the aerogel that drying is produced, partial particulate is in fact xerogel.Meanwhile, drying means is also supercritical drying or general constant pressure and dry process mostly.And realize sensu lato aerogel, aerogel porosity be increased, realize the material of gas distribution at gel skeleton, need the hole remained intact.The finished product simultaneously produced, do not possessing in hydrophobic nature situation, its performance easily affects by extraneous factor, and lose some key propertys, such as heat-proof quality, can reduce the effect of heat insulation of aerogel material itself after water suction, thus limits the widespread use in the heat insulation field of material.
Water glass is a kind of starting material of silica dioxide gel of cheapness, compared to tetraethoxy, methyl silicate, the material cost such as poly silicon are cheap, and configuration can adopt the known method of art technology can be just realize water glass solution configuration, the system that water glass solution adopts simultaneously is the aqueous solution, compared to other silicon sources, as tetraethoxy, the alcoholic solution system adopted, no matter be economically, or security, all even better but, just because of be water solution system, so want drying to go out sensu lato " aerogel ", need to solve dehydration, the xerogel of aerogel formula is become by wet gel, a kind of special technique is needed to realize.And in the dry technology of bulletin, such as, supercritical drying is a kind of implementation, but because of supercritical drying cost very expensive, and for supercutical fluid, it has certain restricted to solvent, such as supercritical carbon dioxide fluid is difficult to convection drying smoothly to contain the wet gel of large water gaging, which limits the difficulty of convection drying, realize such as will taking multiple treatment measures, such as exchange of solvent, this also undoubtedly in add natively expensive supercritical drying cost.So, be directed to more cheap water glass silicon source and prepare aerogel material, be badly in need of a kind of safe and comparatively economic mode.
Summary of the invention
Based on this, be necessary to provide a kind of and can obtain that cost is low and normal temperature thermal conductivity is little, the preparation method of hydrophobic rate much higher hole aerogel composite.
A preparation method for porous aerogel composite, comprises the steps:
(1) reinforcement is placed in reaction vessel and vacuumizes after sealing;
(2) by mass concentration be 5 ~ 40% water glass solution sucting reaction container in until do not have reinforcement;
(3) pump into sour gas and adjust the temperature to 20 ~ 60 DEG C when pH is 5 ~ 8, leave standstill 0.5 ~ 24h, form wet gel reinforcement mixture, pump into mass concentration be the water phase surfactant mixture of 1 ~ 20% to not having wet gel reinforcement mixture, reaction 1 ~ 72h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in wet gel reinforcement mixture be separated and throws away;
(5) pumping into volume ratio is that the organic solvent of 0.5 ~ 100:1 and the mixed solution of surface-modifying agent are to not having described wet gel reinforcement mixture, after reaction 0.5 ~ 72h, discharge spillage, described organic solvent is water-free ethers, ketone, ester class, alcohols, aliphatic series or aromatic hydrocarbon based, and described surface-modifying agent is reagent, mixture or silane coupling agent for making gel or hydroxyl surface silylation reactive;
(6) heat up, the process of evaporation of residual organic solvent final vacuum, pressure release, to obtain final product.
Wherein in an embodiment, the opalizer containing one or more nano level counter radiation effects in step (2) described water glass solution.
Wherein in an embodiment, the concentration of described opalizer in water glass solution is 0.1 ~ 10%(w/v), be more preferably 1-6%, described opalizer is titanium oxide, carbon black, aluminum oxide, ferric oxide, magnesium oxide.
Wherein in an embodiment, step (3) described sour gas is carbonic acid gas or acetic acid, and described tensio-active agent is anion active agent, and described anion active agent is more preferably sodium laurylsulfonate.
Wherein in an embodiment, step (5) described organic solvent is dehydrated alcohol, acetone, Virahol, methylene dichloride, normal hexane, normal heptane, methyl alcohol, ethyl acetate, fluoroalkane.
Wherein in an embodiment, step (5) described surface-modifying agent is hexamethyldisilazane, hexamethyldisiloxane, Union carbide A-162, dimethyl triethoxyl silane, trimethylchlorosilane, or its any mixture.
Wherein in an embodiment, step (5) described organic solvent is dehydrated alcohol, acetone, normal hexane or methyl alcohol, and described surface-modifying agent is hexamethyldisilazane.
Wherein in an embodiment, the volume ratio of step (5) described organic solvent and surface-modifying agent is 4 ~ 30:1, is more preferably 4 ~ 6:1.
Another object of the present invention is to provide a kind of porous aerogel composite.
Technical scheme is as follows: the porous aerogel composite obtained according to above-mentioned preparation method.
Another object of the present invention is to the application that porous aerogel composite is provided.
Specifically comprise: the application of described porous aerogel composite in lagging material, sorbing material.
Foregoing invention adopts water glass as starting material, and with low cost, production safety coefficient is high, and whole reaction process, not by external interference, improve the stability of the method.
By great many of experiments and the experience of contriver, obtain optimum process of the present invention combination, preparation method of the present invention is simple and practical, and cost is low, and the aerogel material obtained, heat-proof quality is superior, porosity is high, and normal temperature thermal conductivity is low, and the finished product obtained also has good hydrophobicity, hydrophobic rate is high, can be used as the energy-efficient lagging material needed for field of thermal insulation such as industrial pipeline equipment, kiln, building, consumption.Meanwhile, because of its high porosity, adsorptivity is strong, can use as sorbing material in pharmaceutical industry, environmental protection industry (epi), substance adsorber industry.
Embodiment
Embodiment 1
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt fibrous carrier fibrefelt to be prefabricated into 0.5m high, 0.5m coil diameter fibre reinforcement, be then placed in reaction vessel and vacuumize after sealing, vacuum tightness is 1Mpa;
(2) prefabricated water glass solution, described water glass solution mass concentration is 5%, open pump, by prefabricated water glass solution sucting reaction container until do not have fibre reinforcement;
(3) pumping into carbon dioxide to pH is 5, gas is constantly dissolved in water glass solution, adjust the temperature to 20 DEG C of stoppings to pump into, leave standstill 0.5h, until reaction vessel visual window sees that gel no longer flows, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 1wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 6h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) pump into the normal hexane that the volume ratio prepared is 4:1 and being mixed to of hexamethyldisilazane there was not wet gel reinforcement mixture, make mixed solution fully soak wet gel mixture, after soaking reaction 12h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.This aerogel composite, by irregular network structure, have good snappiness, normal temperature thermal conductivity is about below 0.018w/m.k, porosity more than 90%, hydrophobic performance is good, hydrophobic rate is 99%, and chemical stability is good, and conventional means can be used to cut randomly size, its extremely low thermal conductivity gives the effect of heat insulation of material high, can be used as the heat insulation field that lagging material is widely used in industrial pipeline, equipment, fire-fighting, Automobile Transportation industry, building trade, electron trade;
Embodiment 2
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt fibrous carrier fiber block to be prefabricated into fibre reinforcement, the length of described fibre reinforcement is 0.5 meter, and width is 0.3 meter, and felt block fibre reinforcement being pressed into different densities is placed in reaction vessel and vacuumizes after sealing, and vacuum tightness is 1Mpa;
(2) water glass solution of 18% concentration is prepared, and to add ultimate density be volume fraction 1%(w/v) opalizer titanium dioxide, be uniformly mixed and be uniformly dispersed, open pump, water glass solution containing opalizer is sucked the reaction vessel that fiber block is housed, until liquid level exceeds the highest liquid level of fibre reinforcement;
(3) pumping into carbon dioxide to pH is 5.5, gas is constantly dissolved in water glass solution, adjust the temperature to 30 DEG C of stoppings to pump into, leave standstill 1h, until reaction vessel visual window sees that gel no longer flows, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 5wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 1h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) mixed solution of the dehydrated alcohol that the volume ratio prepared is 5:1 and hexamethyldisilazane is pumped into reaction vessel, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, mixed solution is made fully to soak wet gel mixture, after soaking reaction 9h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.This aerogel composite, by irregular network structure, have good intensity, normal temperature thermal conductivity is about below 0.019w/m.k, and hydrophobic performance is good, hydrophobic rate is 99%, porosity more than 90%, chemical stability is good, and planarization is good, can be made into the goods of any shape by usage space, its low thermal conductivity can be used as the heat insulation field that lagging material is widely used in industrial equipments, fire-fighting, Automobile Transportation industry, building trade, electron trade.
Embodiment 3
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt fibrous carrier fibrefelt to be prefabricated into fibre reinforcement, the length of described fibre reinforcement is 1 meter, and width is 0.5 meter, and felt block fibre reinforcement being pressed into different densities is placed in reaction vessel and vacuumizes after sealing, and vacuum tightness is 1Mpa;
(2) water glass solution of 20wt% concentration is prepared, and to add ultimate density be volume fraction 2%(w/v) opalizer carbon black, be uniformly mixed and be uniformly dispersed, open pump, water glass solution containing opalizer is sucked the reaction vessel that fiber needled felt is housed, until liquid level exceeds the highest liquid level of fibre reinforcement;
(3) pumping into carbon dioxide to pH is 6, gas is constantly dissolved in water glass solution, be warming up to 50 DEG C, stopping pumps into, and leaves standstill 2h, until reaction vessel visual window sees that gel no longer flows after boosting, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 5wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 8h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) mixed solution of the acetone that the volume ratio prepared is 6:1 and hexamethyldisilazane is pumped into reaction vessel, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, make mixed solution fully soak wet gel mixture, after soaking reaction 0.5h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.
This aerogel composite, by irregular network structure, have good snappiness, normal temperature thermal conductivity is about below 0.019w/m.k, and hydrophobic performance is good, hydrophobic rate is 99%, porosity more than 90%, chemical stability is good, can well reflect and absorptive thermal radiation under high temperature, the high temperature insulating excellent performance of product, can be widely used in the heat insulation field of industrial pipeline, equipment, fire-fighting, Automobile Transportation industry, building trade, electron trade.
Embodiment 4
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt glass fiber powder to be prefabricated into reinforcement, reinforcement be fixed on after certain grinding tool box to be placed in reaction vessel sealing and vacuumize, vacuum tightness is 1Mpa;
(2) prepare the water glass solution of 20wt% concentration, open pump, water glass solution is sucked the reaction vessel that glass fiber powder reinforcement is housed, until liquid level exceeds the highest liquid level of reinforcement;
(3) pumping into carbon dioxide to pH is 7.0, gas is constantly dissolved in water glass solution, adjust the temperature to 55 DEG C of stoppings to pump into, leave standstill 1h, until reaction vessel visual window sees that gel no longer flows, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 5wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 24h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) mixed solution of the methyl alcohol that the volume ratio prepared is 30:1 and hexamethyldisilazane is pumped into reaction vessel, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, make mixed solution fully soak wet gel mixture, after soaking reaction 48h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.This aerogel composite, be by irregular three-dimensional net structure, porosity more than 90%, specific surface area is about 600m
2/ g, adsorptivity is strong, and chemical stability is good, can be reprocessed into the particulate state of different volumes size, can be applicable to the industries such as pharmaceutical industry, environmental protection industry (epi), substance adsorber as sorbing material.
Embodiment 5
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt fibrous carrier fiber block to be prefabricated into fibre reinforcement, the length of described fibre reinforcement is 1.4 meters, and width is 0.8 meter, and felt block fibre reinforcement being pressed into different densities is placed in reaction vessel and vacuumizes after sealing, and vacuum tightness is 1Mpa;
(2) water glass solution of 28wt% concentration is prepared, and to add ultimate density be volume fraction 4%(w/v) opalizer magnesium oxide, be uniformly mixed and be uniformly dispersed, open pump, water glass solution containing opalizer is sucked the reaction vessel that fiber block is housed, until liquid level exceeds the highest liquid level of fibre reinforcement;
(3) pumping into carbon dioxide to pH is 7.5, gas is constantly dissolved in water glass solution, adjust the temperature to 60 DEG C of stoppings to pump into, leave standstill 10h, until reaction vessel visual window sees that gel no longer flows, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 5wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 72h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) mixed solution of the normal hexane that the volume ratio prepared is 6:1 and hexamethyldisilazane is pumped into reaction vessel, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, make mixed solution fully soak wet gel mixture, after soaking reaction 9h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.This aerogel composite, by irregular network structure, have good intensity, normal temperature thermal conductivity is about below 0.018w/m.k, and hydrophobic performance is good, porosity more than 90%, hydrophobic rate is 99%, and chemical stability is good, and planarization is good, the goods of any shape can be made into by usage space, the heat insulation field of industrial equipments, fire-fighting, Automobile Transportation industry, building trade, electron trade can be widely used in.
Embodiment 6
A preparation method for porous aerogel composite, comprises the steps:
(1) adopt fibrous carrier fiber block to be prefabricated into fibre reinforcement, the length of described fibre reinforcement is 1.0 meters, and width is 0.6 meter, and felt block fibre reinforcement being pressed into different densities is placed in reaction vessel and vacuumizes after sealing, and vacuum tightness is 1Mpa;
(2) water glass solution of 40wt% concentration is prepared, and to add ultimate density be volume fraction 6%(w/v) opalizer aluminum oxide, be uniformly mixed and be uniformly dispersed, open pump, water glass solution containing opalizer is sucked the reaction vessel that fiber block is housed, until liquid level exceeds the highest liquid level of fibre reinforcement;
(3) pumping into carbon dioxide to pH is 8.0, gas is constantly dissolved in water glass solution, adjust the temperature to 50 DEG C of stoppings to pump into, leave standstill 24h, until reaction vessel visual window sees that gel no longer flows, form wet gel reinforcement mixture, pump into the sodium dodecyl sulfate aqueous solution of the 20wt% prepared in advance as tensio-active agent, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, carry out washing reaction 36h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in mixture throw away;
(5) mixed solution of the ethyl acetate that the volume ratio prepared is 4:1 and hexamethyldisilazane is pumped into reaction vessel, until liquid level exceeds the highest liquid level of wet gel reinforcement mixture, mixed solution is made fully to soak wet gel mixture, after soaking reaction 72h, discharge spillage till without fluid;
(6) open the heating unit of reaction vessel, reacting by heating container, the organic solvent remained on material and surface-modifying agent are evaporated completely, stops heating, then reaction unit is vacuumized, pressure release, obtain porous aerogel composite finished product.This aerogel composite, by irregular network structure, have good intensity, normal temperature thermal conductivity is about below 0.019w/m.k, and hydrophobic performance is good, porosity more than 90%, hydrophobic rate is 99%, and chemical stability is good, and planarization is good, the goods of any shape can be made into by usage space, the heat insulation field of industrial equipments, fire-fighting, Automobile Transportation industry, building trade, electron trade can be widely used in.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for porous aerogel composite, is characterized in that, comprises the steps:
(1) reinforcement is placed in reaction vessel and vacuumizes after sealing;
(2) by mass concentration be 5 ~ 40% water glass solution sucting reaction container in until do not have reinforcement;
(3) pump into sour gas and adjust the temperature to 20 ~ 60 DEG C when pH is 5 ~ 8, leave standstill 0.5 ~ 24h, form wet gel reinforcement mixture, pump into mass concentration be the water phase surfactant mixture of 1 ~ 20% to not having wet gel reinforcement mixture, reaction 1 ~ 72h;
(4) rotary motion wet gel reinforcement mixture, makes the liquor in wet gel reinforcement mixture be separated and throws away;
(5) pumping into volume ratio is that the organic solvent of 4 ~ 30:1 and the mixed solution of surface-modifying agent are to not having described wet gel reinforcement mixture, after reaction 0.5 ~ 72h, discharge spillage, described organic solvent is water-free ethers, ketone, ester class, alcohols, aliphatic series or aromatic hydrocarbon based, and described surface-modifying agent is to make the reagent of gel or hydroxyl surface silylation reactive, mixture or silane coupling agent;
(6) heat up, the process of evaporation of residual organic solvent final vacuum, pressure release, to obtain final product.
2. the preparation method of porous aerogel composite according to claim 1, is characterized in that, the opalizer containing one or more nano level counter radiation effects in step (2) described water glass solution.
3. the preparation method of porous aerogel composite according to claim 2, is characterized in that, the concentration of described opalizer in water glass solution is 0.1 ~ 10%w/v, and described opalizer is titanium oxide, carbon black, aluminum oxide, ferric oxide, magnesium oxide.
4. the preparation method of porous aerogel composite according to claim 1, is characterized in that, step (3) described sour gas is carbonic acid gas or acetic acid, and described tensio-active agent is anion active agent.
5. the preparation method of porous aerogel composite according to claim 1, it is characterized in that, step (5) described organic solvent is dehydrated alcohol, acetone, Virahol, methylene dichloride, normal hexane, normal heptane, methyl alcohol, ethyl acetate, fluoroalkane.
6. the preparation method of porous aerogel composite according to claim 1, it is characterized in that, step (5) described surface-modifying agent is hexamethyldisilazane, hexamethyldisiloxane, Union carbide A-162, dimethyl triethoxyl silane, trimethylchlorosilane, or its any mixture.
7. the preparation method of the porous aerogel composite according to claim 5 or 6, is characterized in that, step (5) described organic solvent is dehydrated alcohol, acetone, normal hexane or methyl alcohol, and described surface-modifying agent is hexamethyldisilazane.
8. the porous aerogel composite that the preparation method according to any one of claim 1 ~ 7 obtains.
9. the application of porous aerogel composite according to claim 8 in lagging material, sorbing material.
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| CN103965505B (en) * | 2014-05-15 | 2016-08-17 | 广东埃力生高新科技有限公司 | There is polyimide aerogels of counter infrared ray radiation characteristic and preparation method thereof |
| CN105693240A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Preparation method of germanium oxide-niobium oxide hybrid aerogel composite material |
| CN107417234A (en) * | 2017-09-20 | 2017-12-01 | 中国核动力研究设计院 | Aeroge heat preserving and insulating material with γ irradiation shielding properties and preparation method thereof |
| CN111774018B (en) * | 2020-06-19 | 2022-03-15 | 浙江建业化工股份有限公司 | Plasticizer DOTP energy-saving reaction system of high-efficient edulcoration |
| CN112524889B (en) * | 2020-11-25 | 2022-05-13 | 航天特种材料及工艺技术研究所 | Drying method of light dimensional ablation aerogel material |
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| CN101696101B (en) * | 2009-10-30 | 2012-06-20 | 广东埃力生高新科技有限公司 | Heat-insulating material and preparation method thereof |
| CN101823720A (en) * | 2010-04-27 | 2010-09-08 | 重庆工商大学 | Preparation method of nano silica powder |
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Address after: 513042 District 4, Yinghong Industrial Zone, Yinghong Town, Yingde City, Qingyuan City, Guangdong Province Patentee after: Guangdong Ellison Technology Co.,Ltd. Address before: 513042 District 4, Yinghong Industrial Zone, Yinghong Town, Yingde City, Qingyuan City, Guangdong Province Patentee before: GUANGDONG ALISON HI-TECH Co.,Ltd. |