CN105565397A - Preparation method of germanium oxide and rhodium oxide hybrid aerogel composite material - Google Patents
Preparation method of germanium oxide and rhodium oxide hybrid aerogel composite material Download PDFInfo
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Abstract
The invention provides a preparation method of a germanium oxide and rhodium oxide hybrid aerogel composite material. The method comprises the steps that prepared hybrid aerogel is infiltrated into a treated inorganic fiber material, gelling and sufficient aging are carried out, then supercritical drying is carried out, and finally the hybrid aerogel composite material is obtained. According to the technical scheme, the preparation technology is simple and easy to operate, and the germanium oxide and rhodium oxide hybrid aerogel which is excellent in performance is prepared for the first time; the germanium oxide and rhodium oxide hybrid aerogel has the high specific surface area of 350-450 m<2>/g, the low density of 0.13-0.20 g/m<3>, and the high porosity of 80-90%. The heat conductivity of the aerogel composite material is smaller than 0.035 w/m.k, and the shrinking percentage of the aerogel composite material is smaller than 3.4% under the 1000 DEG C. According to the technical scheme, the development and application of the germanium oxide material are broadened.
Description
Technical field
The present invention relates to a kind of preparation method of aerogel, specifically, relate to the preparation method of a kind of germanium oxide and rhodium oxide aerogel composite.
Background technology
Aerogel refers to assembles the nanoporous network of formation for skeleton mutually with nano particle, and in network skeleton hole, be full of the lightweight nano solid material of gaseous state dispersion medium.Aerogel is as a kind of nano material, except the characteristic with nano material, also there are other excellent properties, as: high porosity, high-specific surface area, extremely low density, low thermal conductivity and low sound transmission speed etc., have huge application prospect in catalysis, space flight, medicine, the energy, building and metallurgy etc.
Meanwhile, aerogel kind have also been obtained extreme enrichment, and as metal aerogel, organic aerogel and carbon aerogels, so far increasing Novel air gel is progressively developed.
Germanium oxide can be widely used in and make high pure metal germanium, germanium compound, chemical catalyst, medicine industry, PET resin, electron device etc.; Such as, the glass containing germanium oxide has higher specific refractory power and dispersion, can be used as pantoscope and microscope camera lens.In order to expand the development of aerogel further, the present invention has the germanium oxide of unique texture and performance and the preparation method of rhodium oxide hybrid aerogel matrix material by setting forth first, development and the application of such material can better be promoted, widen the kind of aerogel simultaneously, promote the development of aerogel science and technology.
Summary of the invention
The object of this invention is to provide the preparation method of the little germanium oxide of a kind of high-specific surface area, low density, high porosity, low heat conduction and shrinking percentage and rhodium oxide hybrid aerogel matrix material; Technical scheme manufacture craft provided by the invention is simple, easy to operate, and prepares germanium oxide and the rhodium oxide hybrid aerogel of excellent performance first.
Realize the object of the invention technical scheme as follows:
A preparation method for germanium oxide and rhodium oxide hybrid aerogel matrix material, described matrix material comprises germanium oxide and rhodium oxide hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150 ~ 200 DEG C, dry inorganic fibre 4 ~ 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:2 ~ 4:0.004 ~ 0.008:0.012 ~ 0.02 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 1 ~ 3 hour at 160 ~ 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, described inorganic fibre is porous boron nitride nanofiber, and the preparation method of described porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: the proportions mixed solution by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer according to mol ratio being 0.5 ~ 1:0.5 ~ 2:10 ~ 50:10 ~ 40:0.05 ~ 0.5:10-4 ~ 10-2, after stirring 10 ~ 20min leaves standstill, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 20 ~ 50 DEG C of aging 20 ~ 50h, after ethanol or CO 2 supercritical drying; Under protection of inert gas, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and rhodium oxide hybrid aerogel matrix material.
Further, described step 4) in rare gas element be nitrogen, helium or neon.Described step 4) in high-temperature calcination temperature be 600 ~ 1200 DEG C.
Further, described alcohols material is methyl alcohol, ethanol, propyl alcohol or butanols.Described catalyzer is hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, oxalic acid or hydrofluoric acid.Described coupling agent is γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, methyltrimethoxy silane or vinyltrimethoxy silane.Described tensio-active agent is dodecyl benzyl dimethyl ammonium chloride, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether.
Further, the germanium oxide prepared of described method and rhodium oxide hybrid gel specific surface area 350 ~ 450m
2/ g, porosity 80 ~ 90%.The germanium oxide that described method is prepared and the thermal conductivity of rhodium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme preparation technology provided by the invention is simple, easy to operate, is applicable to scale operation, and prepares germanium oxide and the rhodium oxide hybrid aerogel of excellent performance first.
2, technical scheme provided by the invention prepares high-specific surface area, low density, the germanium oxide of high porosity and rhodium oxide hybrid aerogel, and its excellent properties is specific surface area 350 ~ 450m
2/ more than g, density 0.13 ~ 0.20g/m
3, porosity 80 ~ 90%.
3, the germanium oxide prepared of technical scheme provided by the invention and the thermal conductivity of rhodium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
4, technical scheme provided by the invention, has widened development and the application of germanium oxide material.
Embodiment
Further be clearly and completely described technical scheme below in conjunction with the embodiment of the present invention, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, all belongs to the scope of protection of the invention.
Embodiment 1
1) process of inorganic fibers: at 200 DEG C, dry inorganic fibre 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:4:0.008:0.02 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 1 hour at 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 1:0.5:10:10:0.05:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 80 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 50 DEG C of aging 20h, after supercritical drying; Under inert nitrogen gas protection, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 600 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
Embodiment 2
1) process of inorganic fibers: at 150 DEG C, dry inorganic fibre 6 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:2:0.004:0.012 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 160 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 0.5:2:50:40:0.5:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 50 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 20 DEG C of aging 50h, after ethanol or CO 2 supercritical drying; Under the protection of rare gas element neon, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 1200 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
Embodiment 3
1) process of inorganic fibers: at 180 DEG C, dry inorganic fibre 5 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.006:0.016 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 2 hours at 200 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 1::30:20:0.1:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 20min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 70 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 40 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 800 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
Embodiment 4
1) process of inorganic fibers: at 180 DEG C, dry inorganic fibre 4 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.007:0.014 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 180 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 0.5:1:40:30:0.2:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4proportions mixed solution, stir 15min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 45 DEG C of aging 30h, after ethanol or CO 2 supercritical drying; Under inert nitrogen gas protection, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 900 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
Embodiment 5
1) process of inorganic fibers: at 175 DEG C, dry inorganic fibre 4 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:4:0.007:0.018 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 2 hours at 220 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 1:2:35:25:0.4:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-2proportions mixed solution, stir 18min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 75 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 40 DEG C of aging 45h, after ethanol or CO 2 supercritical drying; Under the protection of rare gas element neon, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 1000 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
Embodiment 6
1) process of inorganic fibers: at 200 DEG C, dry inorganic fibre 5 hours; Inorganic fibre is immersed after being the surface treatment agent solution of the proportions of 1:3:0.006:0.016 by inorganic fibre, distilled water, tensio-active agent and coupling agent weight ratio, dry 3 hours at 200 DEG C, cool to obtain the inorganic fibre after surface treatment;
Wherein, inorganic fibre is porous boron nitride nanofiber, and the preparation method of porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 1:2:35:40:0.5:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-3proportions mixed solution, stir 14min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; After 25 DEG C of aging 35h, after ethanol or CO 2 supercritical drying; Under inert gas helium protection, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out 1100 DEG C of high-temperature calcinations, obtains germanium oxide and rhodium oxide hybrid aerogel matrix material.
The raw materials used kind of the various embodiments described above and ratio thereof, as shown in table 1.
Table 1
In embodiment, gained properties of sample is listed in the table below 2.
Table 2
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent to replace, these do not depart from any amendment of spirit and scope of the invention or equivalently to replace within the claims that all awaits the reply in application.
Claims (9)
1. a preparation method for germanium oxide and rhodium oxide hybrid aerogel matrix material, is characterized in that, described matrix material comprises germanium oxide and rhodium oxide hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150 ~ 200 DEG C, dry inorganic fibre 4 ~ 6 hours; After inorganic fibre is immersed the surface treatment agent solution process of preparing by weight the inorganic fibre of ratio be 1:2 ~ 4:0.004 ~ 0.008:0.012 ~ 0.02, distilled water, tensio-active agent and coupling agent, dry 1 ~ 3 hour at 160 ~ 220 DEG C, cooling;
Wherein, described inorganic fibre is porous boron nitride nanofiber, and the preparation method of described porous boron nitride nanofiber comprises: with boric acid and trimeric cyanamide for raw material, Hydrothermal Synthesis melamine hypoboric acid precursor powder; Adopt freeze-drying, by the liquid nitrogen quick freeze cooling of the hydrothermal solution of melamine hypoboric acid presoma, subsequent drying, makes melamine hypoboric acid nanofiber; Under protective atmosphere, high temperature pyrolysis melamine hypoboric acid nanofiber obtains porous boron nitride nanofiber;
2) preparation of germanium oxide and rhodium oxide hybrid collosol: be 0.5 ~ 1:0.5 ~ 2:10 ~ 50:10 ~ 40:0.05 ~ 0.5:10 according to mol ratio by germanium chloride, rhodium chloride, alcohols material, deionized water, propylene oxide and catalyzer
-4~ 10
-2proportions mixed solution, stir 10 ~ 20min leave standstill after, obtain germanium oxide and rhodium oxide hybrid collosol;
3) infiltrate: by step 2) germanium oxide and the infiltration of rhodium oxide hybrid collosol through step 1) inorganic fibers after process;
4) prepare germanium oxide and rhodium oxide hybrid aerogel matrix material: at 50 ~ 80 DEG C, make step 3) gained infiltration thing in germanium oxide and rhodium oxide hybrid collosol generation gelling, obtain germanium oxide and rhodium oxide hybrid gel; At 20 ~ 50 DEG C after aging 20 ~ 50h, after ethanol or CO 2 supercritical drying; Under protection of inert gas, germanium oxide and rhodium oxide hybrid aerogel matrix material are carried out high-temperature calcination, obtain germanium oxide and rhodium oxide hybrid aerogel matrix material.
2. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, is characterized in that, described step 4) in rare gas element be nitrogen, helium or neon.
3. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, is characterized in that, described step 4) in high-temperature calcination temperature be 600 ~ 1200 DEG C.
4. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, is characterized in that, described alcohols material is methyl alcohol, ethanol, propyl alcohol or butanols.
5. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, is characterized in that, described catalyzer is hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid, oxalic acid or hydrofluoric acid.
6. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, it is characterized in that, described coupling agent is γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, methyltrimethoxy silane or vinyltrimethoxy silane.
7. the preparation method of a kind of germanium oxide as claimed in claim 1 and rhodium oxide hybrid aerogel matrix material, it is characterized in that, described tensio-active agent is dodecyl benzyl dimethyl ammonium chloride, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether.
8., as the germanium oxide of claim 1 ~ 7 as described in any one and the preparation method of rhodium oxide hybrid aerogel matrix material, it is characterized in that, germanium oxide prepared by described method and rhodium oxide hybrid gel specific surface area 350 ~ 450m
2/ g, porosity 80 ~ 90%.
9. as the germanium oxide of claim 1 ~ 7 as described in any one and the preparation method of rhodium oxide hybrid aerogel matrix material, it is characterized in that, the germanium oxide that described method is prepared and the thermal conductivity of rhodium oxide hybrid aerogel matrix material at 1000 DEG C are less than 0.035w/mk, and shrinking percentage is less than 3.4%.
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| CN113754422A (en) * | 2020-06-01 | 2021-12-07 | 厦门稀土材料研究所 | Porous high-entropy rare earth ferrite ceramic material and preparation method and application thereof |
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