CN105693216A - Preparation method of germanium oxide-cadmium oxide hybrid aerogel composite material - Google Patents
Preparation method of germanium oxide-cadmium oxide hybrid aerogel composite material Download PDFInfo
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Abstract
The invention provides a preparation method of a germanium oxide-cadmium oxide hybrid aerogel composite material. The method comprises the following steps: impregnating a prepared hybrid sol into a treated inorganic fiber material, carrying out gelation and sufficient aging, and carrying out supercritical drying with ethanol or carbon dioxide, thereby obtaining the hybrid aerogel composite material. The preparation technique provided by the technical scheme is simple and easy to operate, and can be used for preparing the germanium oxide-cadmium oxide hybrid aerogel with excellent properties for the first time. The high-specific-area low-density high-porosity germanium oxide-cadmium oxide hybrid aerogel prepared by the technical scheme has excellent properties: the specific area is 350-450 m<2>/g, the density is 0.13-0.20 g/m<3>, and the porosity is 70-80%. The thermal conductivity of the aerogel composite material at 1000 DEG C is less than 0.035 W/m.K, and the shrinkage is less than 3.4%. The technical scheme provided by the invention widens the development and application range of the germanium oxide material.
Description
Technical field
The preparation method that the present invention relates to a kind of aeroge, specifically, relates to a kind of germanium oxide and the preparation method of Aska-Rid. aerogel composite。
Background technology
Aeroge refers to that the nanoporous network mutually assembling composition with nano-particle is skeleton, and is full of the lightweight nano solid material of gaseous state disperse medium in network skeleton hole。Aeroge 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., in catalysis, space flight, medicine, the energy, building and metallurgy etc., there is huge application prospect。
Meanwhile, aeroge kind have also been obtained extreme enrichment, and such as metal aerogel, organic aerogel and carbon aerogels, so far increasing Novel air gel is progressively developed。
Germanium oxide can be widely used for making high pure metal germanium, germanium compound, chemical catalyst, medical industry, PET resin, electronic device etc.;Such as, the glass containing germanium oxide has higher refractive index and dispersion, can as pantoscope and microscope camera lens。In order to expand the development of aeroge further, the present invention will set forth have the germanium oxide of unique texture and performance and the preparation method of Aska-Rid. hybrid aerogel composite first, can better promote development and the application of such material, widen the kind of aeroge simultaneously, promote the development of aeroge science and technology。
Summary of the invention
The preparation method that it is an object of the invention to provide the little germanium oxide of a kind of high-specific surface area, low-density, high porosity, low heat conduction and shrinkage factor and Aska-Rid. hybrid aerogel composite;Technical scheme processing technology provided by the invention simply, easily operate, and prepares germanium oxide and the Aska-Rid. hybrid aerogel of excellent performance first。
Realize the object of the invention technical scheme as follows:
The preparation method of a kind of germanium oxide and Aska-Rid. hybrid aerogel composite, described composite includes germanium oxide and Aska-Rid. hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150~200 DEG C, dry inorfil 4~6 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:2~4:0.004~0.008:0.012~0.02, dry 1~3 hour at 160~220 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, described inorfil is resurrection glass fibre, and described resurrection glass fibre includes following component by mass percentage: SiO2,50~60%;Na2O, 30~40%;Al2O3,1~10%;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst according to the proportions mixed liquor that mol ratio is 0.5~1:0.5~2:10~50:10~40:0.05~0.5:10-4~10-2, stirring 10~20min obtains germanium oxide and Aska-Rid. hybrid collosol after standing;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 50~80 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 20~50 DEG C of aging 20~50h, after ethanol or carbon dioxide supercritical fluid drying;Under inert gas shielding, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out high-temperature calcination, obtain germanium oxide and Aska-Rid. hybrid aerogel composite。
Further, described step 4) in noble gas be nitrogen, helium or neon。Described step 4) in high-temperature calcination temperature be 600~1200 DEG C。
Further, described alcohols material is methanol, ethanol, propanol or butanol。Described catalyst is hydrochloric acid, sulphuric acid, phosphoric acid, formic acid, acetic acid, ethanedioic acid or Fluohydric acid.。Described coupling agent is gamma-aminopropyl-triethoxy-silane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, MTMS or vinyltrimethoxy silane。Described surfactant is dodecyl dimethyl benzyl ammonium chloride, dodecylbenzene sodium sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether。
Further, the germanium oxide that prepared by described method and Aska-Rid. hybrid gel specific surface area 350~450m2/ g, porosity 70~80%。Germanium oxide that described method is prepared and Aska-Rid. hybrid aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor 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 simply, easily operate, and is suitable for large-scale production, and prepares germanium oxide and the Aska-Rid. 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 Aska-Rid. hybrid aerogel, and its excellent properties is specific surface area 350~450m2/ more than g, density 0.13~0.20g/m3, porosity 70~80%。
3, technical scheme provided by the invention is prepared germanium oxide and Aska-Rid. hybrid aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor is less than 3.4%。
4, technical scheme provided by the invention, has widened development and the application of germanium oxide material。
Detailed description of the invention
Further technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments。Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, broadly fall into the scope of protection of the invention。
Embodiment 1
1) process of inorganic fibers: at 200 DEG C, dry inorfil 6 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:4:0.008:0.02, dry 1 hour at 220 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 1:0.5:10:10:0.05:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-4Proportions mixed liquor, stirring 20min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 80 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 50 DEG C of aging 20h, after supercritical drying;Under inert nitrogen gas is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 600 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
Embodiment 2
1) process of inorganic fibers: at 150 DEG C, dry inorfil 6 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:2:0.004:0.012, dry 3 hours at 160 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 0.5:2:50:40:0.5:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-2Proportions mixed liquor, stirring 15min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 50 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 20 DEG C of aging 50h, after ethanol or carbon dioxide supercritical fluid drying;Under noble gas neon is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 1200 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
Embodiment 3
1) process of inorganic fibers: at 180 DEG C, dry inorfil 5 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.006:0.016, dry 2 hours at 200 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 1::30:20:0.1:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-3Proportions mixed liquor, stirring 20min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 70 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 40 DEG C of aging 35h, after ethanol or carbon dioxide supercritical fluid drying;Under inert gas helium is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 800 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
Embodiment 4
1) process of inorganic fibers: at 180 DEG C, dry inorfil 4 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.007:0.014, dry 3 hours at 180 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 0.5:1:40:30:0.2:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-4Proportions mixed liquor, stirring 15min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 45 DEG C of aging 30h, after ethanol or carbon dioxide supercritical fluid drying;Under inert nitrogen gas is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 900 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
Embodiment 5
1) process of inorganic fibers: at 175 DEG C, dry inorfil 4 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:4:0.007:0.018, dry 2 hours at 220 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 1:2:35:25:0.4:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-2Proportions mixed liquor, stirring 18min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 75 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 40 DEG C of aging 45h, after ethanol or carbon dioxide supercritical fluid drying;Under noble gas neon is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 1000 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
Embodiment 6
1) process of inorganic fibers: at 200 DEG C, dry inorfil 5 hours;After inorfil is immersed the surface treatment agent solution by inorfil, distilled water, surfactant and proportions that coupling agent weight ratio is 1:3:0.006:0.016, dry 3 hours at 200 DEG C, cool down to obtain inorfil after surface treatment;
Wherein, inorfil is resurrection glass fibre;
2) preparation of germanium oxide and Aska-Rid. hybrid collosol: be 1:2:35:40:0.5:10 according to mol ratio by germanium chloride, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-3Proportions mixed liquor, stirring 14min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 65 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;After 25 DEG C of aging 35h, after ethanol or carbon dioxide supercritical fluid drying;Under inert gas helium is protected, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out 1100 DEG C of high-temperature calcinations, obtains germanium oxide and Aska-Rid. hybrid aerogel composite。
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 example is only in order to illustrate that technical scheme is not intended to limit; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention。
Claims (9)
1. the preparation method of a germanium oxide and Aska-Rid. hybrid aerogel composite, it is characterised in that described composite includes germanium oxide and Aska-Rid. hybrid aerogel, inorganic fibers, and described preparation method comprises the steps:
1) process of inorganic fibers: at 150~200 DEG C, dry inorfil 4~6 hours;Inorfil is immersed after processing by weight the surface treatment agent solution for the preparation of the inorfil of ratio of 1:2~4:0.004~0.008:0.012~0.02, distilled water, surfactant and coupling agent, dry 1~3 hour at 160~220 DEG C, cooling;
Wherein, described inorfil is resurrection glass fibre, and described resurrection glass fibre includes following component by mass percentage: SiO2,50~60%;Na2O, 30~40%;Al2O3,1~10%;
2) preparation of germanium oxide and Aska-Rid. 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, Caddy (Cleary), alcohols material, deionized water, expoxy propane and catalyst-4~10-2Proportions mixed liquor, stirring 10~20min stand after, obtain germanium oxide and Aska-Rid. hybrid collosol;
3) infiltration: by step 2) germanium oxide and Aska-Rid. hybrid collosol infiltrate through step 1) process after inorganic fibers;
4) prepare germanium oxide and Aska-Rid. hybrid aerogel composite: at 50~80 DEG C, make step 3) gained infiltration thing in germanium oxide and Aska-Rid. hybrid collosol generation gelling, obtain germanium oxide and Aska-Rid. hybrid gel;At 20~50 DEG C after aging 20~50h, after ethanol or carbon dioxide supercritical fluid drying;Under inert gas shielding, germanium oxide and Aska-Rid. hybrid aerogel composite are carried out high-temperature calcination, obtain germanium oxide and Aska-Rid. hybrid aerogel composite。
2. the preparation method of a kind of germanium oxide as claimed in claim 1 and Aska-Rid. hybrid aerogel composite, it is characterised in that described step 4) in noble gas be nitrogen, helium or neon。
3. the preparation method of a kind of germanium oxide as claimed in claim 1 and Aska-Rid. hybrid aerogel composite, it is characterised 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 Aska-Rid. hybrid aerogel composite, it is characterised in that described alcohols material is methanol, ethanol, propanol or butanol。
5. the preparation method of a kind of germanium oxide as claimed in claim 1 and Aska-Rid. hybrid aerogel composite, it is characterised in that described catalyst is hydrochloric acid, sulphuric acid, phosphoric acid, formic acid, acetic acid, ethanedioic acid or Fluohydric acid.。
6. the preparation method of a kind of germanium oxide as claimed in claim 1 and Aska-Rid. hybrid aerogel composite, it is characterized in that, described coupling agent is gamma-aminopropyl-triethoxy-silane, N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, MTMS or vinyltrimethoxy silane。
7. the preparation method of a kind of germanium oxide as claimed in claim 1 and Aska-Rid. hybrid aerogel composite, it is characterized in that, described surfactant is dodecyl dimethyl benzyl ammonium chloride, dodecylbenzene sodium sulfonate, dimethyl dodecyl amine oxide, dodecyl-dimethyl amine second lactone or glycerin polyoxyethylene ether。
8. such as the preparation method of the claim 1~7 germanium oxide as described in any one and Aska-Rid. hybrid aerogel composite, it is characterised in that germanium oxide prepared by described method and Aska-Rid. hybrid gel specific surface area 350~450m2/ g, porosity 70~80%。
9. such as the preparation method of the claim 1~7 germanium oxide as described in any one and Aska-Rid. hybrid aerogel composite, it is characterized in that, germanium oxide that described method is prepared and Aska-Rid. hybrid aerogel composite thermal conductivity at 1000 DEG C are less than 0.035w/m k, and shrinkage factor is less than 3.4%。
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CN104941538A (en) * | 2015-06-03 | 2015-09-30 | 金承黎 | In-situ composite silicon-based multibasic oxide oxide aerogel material and preparation method thereof |
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