CN101654349B - Method for preparing silica aerogel by doped brucite fiber and titanium dioxide powder - Google Patents
Method for preparing silica aerogel by doped brucite fiber and titanium dioxide powder Download PDFInfo
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- CN101654349B CN101654349B CN 200910067520 CN200910067520A CN101654349B CN 101654349 B CN101654349 B CN 101654349B CN 200910067520 CN200910067520 CN 200910067520 CN 200910067520 A CN200910067520 A CN 200910067520A CN 101654349 B CN101654349 B CN 101654349B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
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- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0004—Compounds chosen for the nature of their cations
- C04B2103/001—Alkaline earth metal or Mg-compounds
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention provides a method for preparing silica aerogel by doped brucite fiber and titanium dioxide powder. The raw materials are available and non-toxic, the doped brucite fiber is used for enhancing the strength of the aerogel, brucite fiber is the only one environmentally friendly fiber which is not cancerogenic at present, fusing point thereof is as high as 1960 DEG C, and the brucite fiber can resist higher temperature compared with glass fiber and the like; the titanium dioxide powder is added, so that the defect of high temperature infrared transparence is avoided and heat conductivity at high temperature can be reduced; and supercritical technology is adopted to prepare aerogel composite material block without crack, the density thereof is 0.13-0.3g/cm<3>, heat conductivity at 900K can be reduced to 0.045W.m<-1>.K<-1>, and breaking strength can reach 1.08MPa.
Description
Technical field
The invention belongs to the super insulating material field, be specifically related to prepare the method for the silica aerogel of doping brucite fiber and titania powder.
Background technology
Gas gel is by colloidal particle or high-polymer molecular mutual coalescence formation nanoporous reticulated structure, and in hole, is full of a kind of high dispersive solid-state material of gaseous state dispersion medium, and its solid phase and pore texture are nanometer scale.It is a kind of novel nanometer, porous, low density, amorphous material, has the continuous three-dimensional network structure, and typical network diameter is nano level, because its translucent color and extra light weight also are known as " solid-state cigarette " sometimes.This material seems fragile can't bear; But because its nanoporous network structure has effectively suppressed solid-state, gaseous state and radiation thermal conduction; In fact very sturdy and durable, high energy bears 1400 ℃ high temperature, is the heat insulation heat insulation material of a kind of efficient lightweight nanoporous; Its specific refractory power is also very low in addition, and heat insulation capacity also is eager to excel 39 times than best spun glass.Its structural uniqueness shows a lot of unique character of gas gel and tempting application prospect, has caused chemist, physicist, material scholar's etc. great attention.It shows good using value in fields such as calorifics, optics, electricity, acoustics, mechanics and fractal; In application facet, it has been applied to Cerenkov detector, specific acoustic resistance coupling material, catalyzer and carrier, high efficiency heat insulation material and has prepared efficient rechargeable cell etc.All used SiO on Russia " peace " number space station and the U.S. " Mars Pathfinder " detector
2Gas gel.
Single aerosil is because of some defectives of its existence, and like poor toughness, more crisp, intensity is low, frangible, and has an infrared transparent property during high temperature, and unmodified gas gel is prone to the hydrophilic gel that causes and subsides, limited its practical value.The present invention prepares the fiber reinforcement type gas gel, can improve 2～30 times of intensity, moreover also can improve its toughness.This fiber is an environmental protection fiber, is unique not carcinogenic fiber.And the fusing point height can be high temperature resistant.For reducing the thermal conductivity titania-doped ultra-micro powder of gas gel when the high temperature as opalizer, with blocks infrared radiation.Carry out hydrophobically modified at last, make the surface hydrophilic base become hydrophobic group and reach hydrophobic effect, through the above effort use value of enhanced gas gel greatly.What the present invention selected for use is that nontoxic, cheap industry silicasol is the silicon source, can reduce production costs greatly.Non-pressure process is difficult to prepare the low-density gas gel of flawless, and the employing supercritical process can be prepared and not ftracture, the well behaved aerogel block body of flawless.(reference M Gronauer, J Fricke.Acoustic properties of microporous SiO
2Aerogel.Acustica, 1986,59:177)
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the silica aerogel of doping brucite fiber and titania powder, its step and condition are following:
1) get zero(ppm) water and tensio-active agent and join in the reactor B, be stirred to surfactant dissolves, add brucite fiber again, stirred 20～30 minutes, ultra-sonic oscillation are 10～15 minutes then; Described zero(ppm) water volume ml: tensio-active agent quality g: brucite fiber quality g is 2.7～4.0: 0.0387～0.0637: 0.2655～0.4250; Described tensio-active agent is sodium lauryl sulphate or sodium laurylsulfonate;
2) get zero(ppm) water and place reactor A, constantly stir the adding industry silicasol, join USP Kosher and titania powder in the reactor A in order, drip absolute ethyl alcohol again, dripping speed is 1 droplet/second; When the ethanol in reactor A drips the material in the reactor B is joined in the reactor A, leave standstill gel after stirring; Described zero(ppm) water volume ml: industry silicasol volume ml: USP Kosher volume ml: titania powder quality g: absolute ethyl alcohol volume ml is 2.5～4.5: 10～15: 1～3: 0.8～1.8: 25～30; Described industry silicasol is the JN-30 type, and the silicon-dioxide quality mark in the industry silicasol is 30%, and its pH value 9.0～10.0, density are 1.19～1.21g/cm
3
3) ageing is 2～3 days, for preventing the gel cracking, in reactor A, pours absolute ethyl alcohol protection gel into, and the absolute ethyl alcohol liquid level will not have gel, and with preservative film sealed reactor A;
4) at 30～45 ℃, water: the absolute ethyl alcohol volume ratio is 1: 4～1: 5 composition aged solution, wears out the aged gel of step 3) two days, and the centre is changed aged solution one time;
5) gel after will wearing out is poured in the reactor drum gently, invades bubble 6～10 days with absolute ethyl alcohol, changes in the reactor drum absolute ethyl alcohol every day once;
6) gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 8～1: 10 hydrophobic sol carried out hydrophobically modified 12～15 hours, cleans gel surface with absolute ethyl alcohol again;
7) gel after will cleaning is immersed in the watch-glass and fills it up with ethanol, is put in the extraction kettle, then at 5～10 ℃, soaks 3～5 days with liquid carbon dioxide under 5～8MPa, and emits the ethanol of replacing out; Be warming up to 35～40 ℃ then, 10.5～12.5MPa keeps 3～5h, then with the slow pressure release of speed of 0.35～0.5MPa/h to normal pressure, the silica aerogel block of obtain mixing brucite fiber and titania powder.
Beneficial effect: a kind of method for preparing the silica aerogel of doping brucite fiber and titania powder provided by the invention; Raw material is cheap, nontoxicity, and the doping brucite fiber strengthens the intensity of gas gel; Brucite fiber is present unique not carcinogenic environmental protection fiber; And fusing point is high, is 1960 ℃, than the higher temperature of abilities such as spun glass; Add titania powder and improved the transparent shortcoming of its high-temperature infrared, the thermal conductivity in the time of can reducing high temperature; Adopt supercritical process to prepare flawless bulk aerogel composite, its density is 0.13～0.3g/cm
3, thermal conductivity can be low to moderate 0.045Wm during 900K
～1K
～1, folding strength can reach 1.08Mpa.
Description of drawings
Fig. 1 is the stereoscan photograph of the silica aerogel of doping brucite fiber and titania powder.
Embodiment
Embodiment 1
Measure 3.8ml zero(ppm) water in beaker B, weighing 0.0398g sodium laurylsulfonate joins among the beaker B, stirs and causes its dissolving, adds the 0.2655g brucite fiber again, stirs 30 minutes, and ultra-sonic oscillation are 10 minutes then; Measure 4ml zero(ppm) water in beaker A, constantly stir adding 15ml industry silicasol, measure the 3ml USP Kosher again and join among the beaker A, add the 1.8g titania powder, drip the 30ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 2 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; 45 ℃ of following waters: the absolute ethyl alcohol volume ratio is that 1: 5 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 6 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 10 hydrophobic sol carried out hydrophobically modified 12 hours, cleans gel surface with absolute ethyl alcohol again; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 3 days with liquid carbon dioxide under the 7MPa, and emit the ethanol that displaces then at 8 ℃; Be warming up to 38 ℃ then, 11MPa, and keep 3h, then with the slow pressure release of speed of 0.35MPa/h to normal pressure, obtain aerogel block body.Density is 0.25g/cm
3, specific surface area is 755m
2/ g, voidage is 92.3%.
Embodiment 2
Measure 4.0ml zero(ppm) water in beaker B, weighing 0.0637g sodium laurylsulfonate joins among the beaker B, stirs and causes its dissolving, adds the 0.4250g brucite fiber again, stirs 20 minutes, and ultra-sonic oscillation are 13 minutes then; Measure 4.5ml zero(ppm) water in beaker A, constantly stir adding 10ml industry silicasol, measure the 1ml USP Kosher again and join among the beaker A, add the 1.2g titania powder, drip the 29ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 3 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; 30 ℃ of following waters: the absolute ethyl alcohol volume ratio is that 1: 4 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 10 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 8 hydrophobic sol carried out hydrophobically modified 15 hours, cleans gel surface with absolute ethyl alcohol again; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 3 days with liquid carbon dioxide under the 8MPa, and emit the ethanol that displaces then at 10 ℃; Be warming up to 36 ℃ then, 12.5MPa also keeps 5h, then with the slow pressure release of speed of 0.45MPa/h to normal pressure, promptly obtain aerogel block body.Density is 0.31g/cm
3, specific surface area is 719m
2/ g, voidage is 91.4%.
Embodiment 3
Measure 2.8ml zero(ppm) water in beaker B, weighing 0.0387g sodium lauryl sulphate joins among the beaker B, stirs and causes its dissolving, adds the 0.2732g brucite fiber again, stirs 25 minutes, and ultra-sonic oscillation are 10 minutes then; Measure 2.5ml zero(ppm) water in beaker A, constantly stir adding 13ml industry silicasol, measure the 2ml USP Kosher again and join among the beaker A, add the 0.8g titania powder, drip the 27.5ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 2 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; 40 ℃ of following waters: the absolute ethyl alcohol volume ratio is that 1: 4.5 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 10 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 10 hydrophobic sol carried out hydrophobically modified 13 hours, cleans gel surface with absolute ethyl alcohol again; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 3 days with liquid carbon dioxide under the 5MPa, and emit the ethanol that displaces then at 5 ℃; Be warming up to 35 ℃ then, 12MPa also keeps 3h, then with the slow pressure release of speed of 0.5MPa/h to normal pressure, promptly obtain aerogel block body.Density is 0.34g/cm
3, specific surface area is 708m
2/ g, voidage is 90.8%.
Embodiment 4
Measure 2.7ml zero(ppm) water in beaker B, weighing 0.0625g sodium lauryl sulphate joins among the beaker B, stirs and causes its dissolving, adds the 0.4026g brucite fiber again, stirs 30 minutes, and ultra-sonic oscillation are 15 minutes then; Measure 3.5ml zero(ppm) water in beaker A, constantly stir adding 15ml industry silicasol, measure the 2.8ml USP Kosher again and join among the beaker A, add the 1.8g titania powder, drip the 25ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 2.5 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; Water under 35 ℃: the absolute ethyl alcohol volume ratio is that 1: 5 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 8 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 9 hydrophobic sol carried out hydrophobically modified 14 hours, cleans gel surface with absolute ethyl alcohol again; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 4 days with liquid carbon dioxide under the 6.3MPa, and emit the ethanol that displaces then at 5 ℃; Be warming up to 40 ℃ then, 11.5MPa also keeps 4h, then with the slow pressure release of speed of 0.5MPa/h to normal pressure, promptly obtain aerogel block body.Density is 0.22g/cm
3, specific surface area is 815m
2/ g, voidage is 93.7%.
Embodiment 5
Measure 4.0ml zero(ppm) water in beaker B, weighing 0.0532g sodium laurylsulfonate joins among the beaker B, stirs and causes its dissolving, adds the 0.3763g brucite fiber again, stirs 20 minutes, and ultra-sonic oscillation are 15 minutes then; Measure 4.0ml zero(ppm) water in beaker A, constantly stir adding 14ml industry silicasol, measure the 3ml USP Kosher again and join among the beaker A, add the 0.95g titania powder, drip the 30ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 2.5 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; 45 ℃ of following waters: the absolute ethyl alcohol volume ratio is that 1: 4 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 6 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 8 hydrophobic sol carried out hydrophobically modified 12 hours, cleans gel surface with absolute ethyl alcohol again; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 3 days with liquid carbon dioxide under the 7.5MPa, and emit the ethanol that displaces then at 10 ℃; Be warming up to 35 ℃ then, 10.5MPa also keeps 5h, then with the slow pressure release of speed of 0.35MPa/h to normal pressure, promptly obtain aerogel block body.Density is 0.19g/cm
3, specific surface area is 839m
2/ g, voidage is 94.2%.
Embodiment 6
Measure 2.9ml zero(ppm) water in beaker B, weighing 0.0593g sodium lauryl sulphate joins among the beaker B, stirs and causes its dissolving, adds the 0.3879g brucite fiber again, stirs 30 minutes, and ultra-sonic oscillation are 10 minutes then; Measure 3.5ml zero(ppm) water in beaker A, constantly stir adding 10ml industry silicasol, measure the 1ml USP Kosher again and join among the beaker A, add the 1.25g titania powder, drip the 28ml absolute ethyl alcohol again; When the ethanol in beaker A will drip the fiber among the beaker B is joined among the beaker A, leave standstill gel after stirring; Ageing 3 days for preventing cracking, is poured absolute ethyl alcohol protection gel into also with preservative film sealed beaker A in beaker A; Water under 30 ℃: the absolute ethyl alcohol volume ratio is that 1: 5 aged solution wore out two days, and the centre is changed aged solution one time; Gel after aging is poured in the bigger beaker gently, invaded bubble 9 days, change in the beaker absolute ethyl alcohol every day once with absolute ethyl alcohol; Gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 9 hydrophobic sol carried out hydrophobically modified 15 hours, cleans gel surface with absolute ethyl alcohol again; Clean gel surface with absolute ethyl alcohol, prepare dry; Gel is invaded bubble in watch-glass and fill it up with ethanol, be put in the extraction kettle,, soaked 3 days with liquid carbon dioxide under the 8MPa, and emit the ethanol that displaces then at 8 ℃; Be warming up to 37 ℃ then, 11MPa also keeps 4h, then with the slow pressure release of speed of 0.4MPa/h to normal pressure, promptly obtain aerogel block body.Density is 0.27g/cm
3, specific surface area is 832m
2/ g, voidage is 92.9%.
Claims (1)
1. the preparation method of the silica aerogel of doping brucite fiber and titania powder; It is characterized in that; Step and condition are following: 1) get zero(ppm) water and tensio-active agent and join in the reactor B, be stirred to surfactant dissolves, add brucite fiber again; Stirred 20～30 minutes, ultra-sonic oscillation are 10～15 minutes then; Described zero(ppm) water volume ml: tensio-active agent quality g: brucite fiber quality g is 2.7～4.0: 0.0387～0.0637: 0.2655～0.4250; Described tensio-active agent is sodium lauryl sulphate or sodium laurylsulfonate;
2) get zero(ppm) water and place reactor A, constantly stir the adding industry silicasol, join USP Kosher and titania powder in the reactor A in order, drip absolute ethyl alcohol again, dripping speed is 1 droplet/second; When the ethanol in reactor A drips the material in the reactor B is joined in the reactor A, leave standstill gel after stirring; Described zero(ppm) water volume ml: industry silicasol volume ml: USP Kosher volume ml: titania powder quality g: absolute ethyl alcohol volume ml is 2.5～4.5: 10～15: 1～3: 0.8～1.8: 25～30; Described industry silicasol is the JN-30 type, and the silicon-dioxide quality mark in the industry silicasol is 30%, and its pH value 9.0～10.0, density are 1.19～1.21g/cm
3
3) ageing is 2～3 days, for preventing the gel cracking, in reactor A, pours absolute ethyl alcohol protection gel into, and the absolute ethyl alcohol liquid level will not have gel, and with preservative film sealed reactor A;
4) at 30～45 ℃, water: the absolute ethyl alcohol volume ratio is 1: 4～1: 5 composition aged solution, wears out the aged gel of step 3) two days, and the centre is changed aged solution one time;
5) gel after will wearing out is poured in the reactor drum gently, invades bubble 6～10 days with absolute ethyl alcohol, changes in the reactor drum absolute ethyl alcohol every day once;
6) gel is placed trimethylchlorosilane: the normal hexane volume ratio is that 1: 8～1: 10 hydrophobic sol carried out hydrophobically modified 12～15 hours, cleans gel surface with absolute ethyl alcohol again;
7) gel after will cleaning is immersed in the watch-glass and fills it up with ethanol, is put in the extraction kettle, then at 5～10 ℃, soaks 3～5 days with liquid carbon dioxide under 5～8MPa, and emits the ethanol of replacing out; Be warming up to 35～40 ℃ then, 10.5～12.5MPa keeps 3～5h, then with the slow pressure release of speed of 0.35～0.5MPa/h to normal pressure, the silica aerogel block of the sharp titania powder of brucite fiber that obtains mixing.
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| CN106242134A (en) * | 2016-04-21 | 2016-12-21 | 浙江海洋学院 | A kind of oily water purifying treatment method |
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| CN107416848B (en) * | 2017-06-20 | 2019-08-27 | 无锡鸿孚硅业科技有限公司 | A kind of simple preparation method of silica aerogel |
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| CN108435106A (en) * | 2018-03-30 | 2018-08-24 | 齐鲁工业大学 | A kind of preparation method and applications of bulk titanium-based aeroge |
| CN108484094A (en) * | 2018-04-01 | 2018-09-04 | 中鸿纳米纤维技术丹阳有限公司 | A kind of high intensity silica aerogel based on improvement reinforcing material |
| CN109320293A (en) * | 2018-11-16 | 2019-02-12 | 安徽建筑大学 | A kind of modification processing method of hydrophobic nano porous ceramic film material |
| CN113509925B (en) * | 2021-09-07 | 2021-12-03 | 中海油天津化工研究设计院有限公司 | Solid base catalyst and preparation method thereof |
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| US6764543B2 (en) * | 2000-06-22 | 2004-07-20 | Akzo Nobel N.V. | Mixture of silica sols |
| CN1730388A (en) * | 2005-07-12 | 2006-02-08 | 北京科技大学 | Process for preparing stephanoporate powder doped silica aerogel heat-insulation material |
| 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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