CN101696101B - Heat-insulating material and preparation method thereof - Google Patents
Heat-insulating material and preparation method thereof Download PDFInfo
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- CN101696101B CN101696101B CN2009101934794A CN200910193479A CN101696101B CN 101696101 B CN101696101 B CN 101696101B CN 2009101934794 A CN2009101934794 A CN 2009101934794A CN 200910193479 A CN200910193479 A CN 200910193479A CN 101696101 B CN101696101 B CN 101696101B
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Abstract
The invention discloses an aerogel doped meta-titanic acid composite fiber heat-insulating material and a preparation method thereof. The material composition mainly comprises silicon dioxide, a meta-titanic acid serving as a radiation barrier agent and a reinforcing fiber with low stacking density. The weight ratio of the silicon to the meta-titanic acid to the reinforcing fiber is 1:0.1-0.2:1-3. The aerogel doped meta-titanic acid composite fiber heat insulating material can effectively keep out the radiation by introducing meta-titanic acid precipitates in an aerogel by utilizing an in-situ generation method, and avoids the defects of agglomerating the powder radiation barrier agent and improving solid thermal conductivity.
Description
Technical field
The present invention relates to a kind of lagging material and preparation method thereof.
Background technology
At present in heat insulation field; A kind of superinsulation material has appearred; Promptly using aerosil is the fibre-reinforced aerogel matrix material of main heat insulation composition: 1, and the mixture of aerogel particle and fiber is referring to Chinese patent 96196880.X number " aerogel composite that contains fiber ".2, the mixture of aerogel powder and fiber is referring to No. 200510124588.2, Chinese patent " brucite fiber strengthens the preparation method of SIO2 aerogel heat-insulating material ".3, the mixture of continuous gas gel and fiber is referring to No. 200510031952.0, Chinese patent " a kind of aerogel heat-insulating composite material and preparation method thereof ".
The related lagging material of above-mentioned these patented technologies all uses aerosil as heat insulation main raw.Aerosil is because its lower density and nano-pore structure have very strong restraining effect to the convection current in the heat transfer path.Yet at high temperature, for another main path radiation of conducting heat, gas gel can not play good iris action.In fact, for the radiation of near infrared and visible light wave range, gas gel is similar to transparent.In order to address this problem, different patents has adopted different means, and its common ground is to add pulverous radiation resistance barrier material, for example titanium dioxide granule, perhaps carbon black pellet.Yet always there is too big, the pockety shortcoming of particle in Powdered radiation resistance barrier material.No matter be mechanical stirring, still utilize dispersion agent that it is suspended in the colloidal sol gel again, powder inevitably agglomeration can occur, thereby has influenced lagging material for the radiating barriering effect.
After the research of for some time, the contriver notices and can utilize generated in-situ principle that with the compound of titanium, for example in the titanyl sulfate adding sol system, titanyl sulfate can be dissolved in the less water of pH value because of it, thereby is dissolved in the colloidal sol uniformly earlier.After treating its gel, utilize the method that heats up to decompose titanyl sulfate again, just can in gel, generate the metatitanic acid deposition uniformly.The metatitanic acid deposition of white can play the effect of good radiation-inhibiting attached on the gel skeleton, and its dispersive height does not evenly have the agglomeration of powder.
Summary of the invention
The object of the present invention is to provide a kind of lagging material that uses generated in-situ metatitanic acid as opalizer.
The objective of the invention is to realize through following technical scheme:
A kind of gas gel doping metatitanic acid conjugated fibre lagging material, its formation mainly comprises aerosil, radiation barrier agent metatitanic acid, the fiber of enhancing usefulness, three's weight part ratio is 1: 0.1-0.2: 1-3.
Preferably, the fiber of said enhancing usefulness is one or more in spun glass, aluminum silicate fiber, rock wool fibers, pet fiber, the thomel; More preferably, the fiber that uses of said enhancing is spun glass.
Another object of the present invention provides a kind of method for preparing above-mentioned lagging material.
A kind of method for preparing aforesaid lagging material; Mainly comprise the steps: (1) colloidal sol preparation: with the silicon-containing compound is raw material, adds entry as solvent, the content that makes silicon by water be diluted to account for the solution total mass 5% to 20% between; Slowly add an acidic catalyst to aforementioned solution; Add titanyl sulfate afterwards, the amount of adding is 0.133～0.266 times of quality of silicon-containing compound, thereby obtains colloidal sol; (2) make the enhancing body with the fiber that strengthens usefulness: with 0.3 meter to 1.5 meters of fabric width, the inorganic or organic fibre felt that length is 5 meters to 30 meters rolls into the felt volume, as strengthening body; (3) infiltration: (1) gained colloidal sol is immersed in the enhancing body through vacuum impregnation technique; (4) aging: as in 0 ℃-50 ℃, to leave standstill 1 minute-3 days, and waited for that colloidal sol was solidified into gel and aging; (5) hydro-thermal: gel is heated to 80 ℃---120 ℃, to keep 0.5 to 3 hour, the titanium compound in gel decomposes the generation metatitanic acid; (6) washing: the flushing of gel water is lower than 5% until inorganic salt content; (7) displacement: use the carbonatoms that dissolves each other with water less than the water in 16 alcohols, ketone or the ether organic solvent displacement gel; (8) drying: carry out supercritical fluid drying, obtain said lagging material.
Preferably, said silicon-containing compound is a water glass; Said an acidic catalyst is nitric acid or hydrochloric acid or sulfuric acid or phosphoric acid.The carbonatoms that said and water dissolves each other is preferably ethanol less than 16 alcohols, ketone or ether organic solvent.
Said step (1) colloidal sol is formulated as: mass fraction of solids is poured in an acidic catalyst greater than 20% water silicon sol, is 6～7 until pH value.
Perhaps, said step (1) colloidal sol is formulated as: with an acidic catalyst splash into pH value that the pH meter in water glass to the water glass shows be equal to or slightly less than 2.3 obtain the may command gelation rate colloidal sol.
Said Infiltration Technics adopts the way that vacuumizes infiltration, promptly earlier fibre reinforcement is put into vacuum vessel, vacuumizes then, puts into colloidal sol to liquid level and has not just had enhancing body vertex, keeps vacuum for some time, and the venting vacuum gets final product.
It is dry that said supercritical fluid drying can be ethanol or CO 2 supercritical, but be preferably the CO 2 supercritical drying, and the CO 2 supercritical drying has that cost is low, and productive rate is high, and the finished product organic content is few, advantages such as making processes safety.
In the present invention, said original position generate metatitanic acid as the method for radiation barrier agent have barrier agent be evenly distributed, little to the influence of gas gel density, the radiation obstructing capacity is strong, technology is simple, advantage such as with low cost.
Preparing method's simple possible of lagging material of the present invention, excellent property.The lagging material that is prepared by this method has following beneficial effect: (1) adopt generated in-situ way introduce the metatitanic acid deposition as the counter radiation agent, overcome traditional technology and used shortcomings such as reunion that powder causes and density unevenness.Thereby the amount that can control metatitanic acid easily obtains only counter radiation agent addition to different use temperatures.(2) use metatitanic acid as the counter radiation agent, reduced the solid conductive heat of material to a great extent.
Embodiment
Below through embodiment the present invention is described further, but protection domain does not receive the restriction of these embodiment.
Embodiment 1
Silicon water-sol thin up to 20% with mass fraction of solids 40%; Be added dropwise to gradually in the dilute sulphuric acid of massfraction 95% and reach 6.5 until the pH of mixed solution value; In solution, add 0.2 times the titanyl sulfate that is equivalent to solid masses in the silicon water-sol, promptly obtain the silicon dioxide gel of may command gelation rate.The vacuum vessel of uncapping is put into as strengthening body in the felt volume back that the short glass fiber felt is rolled into 0.3 meter of diameter, and the sealing vacuum vessel vacuumizes then, utilizes negative pressure of vacuum to suck colloidal sol to liquid level and has not just had enhancing body vertex, leaves standstill the venting vacuum 5 minutes.Enhancing body after will infiltrating then leaves standstill 1 day (room temperature); Colloidal sol promptly becomes gel and aging; The enhancing body that will be full of gel is subsequently put into heating unit with 105 degrees centigrade steam heating 2 hours, and the titanyl sulfate in the gel promptly takes place to decompose and produces the metatitanic acid deposition, and this moment, gel bleached.To strengthen body afterwards and gel is cooled to room temperature, the water flushing is lower than 5% until inorganic salt content.Again with ethanol exchange water wherein.After exchange is accomplished; To strengthen body and gel is put into autoclave, slowly be warming up to 300 degrees centigrade, and make the still internal pressure reach 12 MPas; Constant temperature after 1 hour slowly relief pressure until still internal pressure and extraneous balance; Open autoclave and take out material, can make gas gel doping metatitanic acid conjugated fibre lagging material, its density is about 0.20g/cm
3, the normal temperature thermal conductivity is about 0.015W/MK.
Embodiment 2
With modulus 3.3; Behind 2 times of the water glass dilute with waters of degree Beaume 30%; Interpolation concentration is that the pH value of the pH meter in 0.05mol/L nitric acid to the water glass is shown as 2.3, in solution, adds 0.15 times the titanyl sulfate that is equivalent to solid masses in the water glass, obtains silica hydrosol.The vacuum vessel of uncapping is put into as strengthening body in the felt volume back that the pet fibre felt is rolled into 0.3 meter of diameter, and the sealing vacuum vessel vacuumizes then, puts into colloidal sol to liquid level and does not have enhancing body vertex, leaves standstill the venting vacuum 5 minutes.Enhancing body after will infiltrating then leaves standstill 1 day (room temperature); Colloidal sol promptly becomes gel; The enhancing body that will be full of gel is subsequently put into heating unit with boiling water (100 degrees centigrade) heating 3 hours, and the titanyl sulfate in the gel promptly takes place to decompose and produces the metatitanic acid deposition, and this moment, gel bleached.To strengthen body afterwards and gel is cooled to room temperature, the water flushing is lower than 5% until inorganic salt content.Again with ethanol exchange water wherein.After exchange is accomplished, will strengthen body and gel is put into autoclave, and utilize carbonic acid gas to carry out supercritical drying; Be about to strengthen body and put into supercritical fluid drying equipment; Vacuumize, pump into supercritical carbon dioxide with pump then, and at equipment the other end Open valve; Emit carbonic acid gas to tripping device with the speed consistent with pump, carbonic acid gas dissolved and carried part ethanol secretly this moment.In tripping device, ethanol and carbon dioxide separation, the carbonic acid gas of separating is pumped in the supercritical fluid drying equipment again, and this process is circulated in the tripping device and can not obtains till the ethanol.The pressure of emptying this moment supercritical fluid drying equipment can make gas gel doping metatitanic acid conjugated fibre lagging material, and its density is about 0.12g/cm
3, the normal temperature thermal conductivity is about 0.012W/MK.
Claims (7)
1. a method for preparing lagging material is characterized in that, comprise the steps: the preparation of (1) colloidal sol: with the silicon-containing compound is raw material; Add entry as solvent; The content that makes silicon by water be diluted to account for the solution total mass 5% to 20% between, slowly add an acidic catalyst to aforementioned solution, add titanyl sulfate afterwards; The amount that adds is 0.133～0.266 times of quality of silicon-containing compound, thereby obtains colloidal sol; (2) fiber that strengthens usefulness is made the enhancing body: with 0.3 meter to 1.5 meters of fabric width, the inorganic or organic fibre felt that length is 5 meters to 30 meters rolls into the felt volume, as strengthening body; (3) infiltration: (1) gained colloidal sol is immersed in the enhancing body through vacuum impregnation technique; (4) aging: as in 0 ℃-50 ℃, to leave standstill 1 minute-3 days, and waited for that colloidal sol was solidified into gel and aging; (5) hydro-thermal: gel is heated to 80 ℃-120 ℃, kept 0.5 to 3 hour, the titanium compound in gel decomposes the generation metatitanic acid; (6) washing: the flushing of gel water is lower than 5% until inorganic salt content; (7) displacement: use the carbonatoms that dissolves each other with water less than the water in 16 alcohols, ketone or the ether organic solvent displacement gel; (8) drying: carry out supercritical fluid drying, obtain said lagging material; Wherein, the silicon-containing compound in said step (1) the colloidal sol preparation is a mass fraction of solids greater than 20% water silicon sol, adds an acidic catalyst, is 6～7 until the pH value.
2. preparation method according to claim 1 is characterized in that, said an acidic catalyst is nitric acid or hydrochloric acid or sulfuric acid or phosphoric acid.
3. preparation method according to claim 1; It is characterized in that; Said step (3) infiltration is: the enhancing body that earlier step (2) is prepared into is put into vacuum vessel, vacuumizes then, utilizes negative pressure of vacuum to suck colloidal sol to liquid level and has not just had enhancing body vertex; Kept vacuum 1 second-1 hour, the venting vacuum gets final product.
4. preparation method according to claim 1 is characterized in that, said supercritical fluid drying is carbonic acid gas or ethanol supercritical drying.
5. preparation method according to claim 1 is characterized in that, the carbonatoms that dissolves each other with water is an ethanol less than 16 alcohols, ketone or ether organic solvent.
6. a lagging material that is obtained by each said preparation method of claim 1-5 is characterized in that, its formation mainly comprises aerosil, radiation barrier agent metatitanic acid, and the fiber of enhancing usefulness, three's weight part ratio is 1: 0.1-0.2: 1-3.
7. lagging material according to claim 6 is characterized in that, said radiation barrier agent metatitanic acid generates gained in gel, utilizing hydrothermal method to decompose the titanyl sulfate original position.
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| CN103524111B (en) * | 2013-10-23 | 2015-06-17 | 广东埃力生高新科技有限公司 | Porous composite aerogel material as well as preparation method and application thereof |
| CN109314200B (en) * | 2016-06-29 | 2022-04-08 | 松下知识产权经营株式会社 | Battery module |
| CN108083835A (en) * | 2017-12-19 | 2018-05-29 | 马斌祥 | A kind of preparation method of antibacterial thermal radiation resistance aeroge |
| CN110080038A (en) * | 2019-03-22 | 2019-08-02 | 嘉兴赛曼泰克新材料有限公司 | High temperature resistant ultrathin low thermal conductivity heat-insulating material and its preparation process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546226A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel and method for making same |
| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN1803602A (en) * | 2005-12-20 | 2006-07-19 | 长安大学 | Method for preparing brucite fiber reinforced SiO2 aerogel heat-insulating material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546226A (en) * | 2003-12-17 | 2004-11-17 | 同济大学 | TiO2/SiO2 aerogel and method for making same |
| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
| CN1803602A (en) * | 2005-12-20 | 2006-07-19 | 长安大学 | Method for preparing brucite fiber reinforced SiO2 aerogel heat-insulating material |
Non-Patent Citations (1)
| Title |
|---|
| 庞颖聪等.TiO2/SiO2气凝胶微球的制备及其表征.《物理化学学报》.2005,第21卷(第12期),全文. * |
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Address after: 513042 Zone 4, Yinghong Industrial Zone, Yinghong Town, Yingde City, Guangdong Province Patentee after: Guangdong Ellison Technology Co.,Ltd. Address before: 513042 Zone 4, Yinghong Industrial Zone, Yinghong Town, Yingde City, Guangdong Province Patentee before: GUANGDONG ALISON HI-TECH Co.,Ltd. |