CN107324348A - A kind of high infrared radiance silicon phosphorus composite aerogel and preparation method thereof - Google Patents

A kind of high infrared radiance silicon phosphorus composite aerogel and preparation method thereof Download PDF

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CN107324348A
CN107324348A CN201710498161.1A CN201710498161A CN107324348A CN 107324348 A CN107324348 A CN 107324348A CN 201710498161 A CN201710498161 A CN 201710498161A CN 107324348 A CN107324348 A CN 107324348A
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preparation
colloidal sol
composite aerogel
silicon phosphorus
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张志杰
邓依依
钟明峰
李娜
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South China University of Technology SCUT
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    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
    • C01B33/1585—Dehydration into aerogels
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    • C01B25/00—Phosphorus; Compounds thereof
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Abstract

The invention discloses a kind of high infrared radiance silicon phosphorus composite aerogel and preparation method thereof, this method utilizes tetraethyl orthosilicate（TEOS）And triethyl phosphate（TEP）For raw material, Ludox and phosphorus colloidal sol are prepared respectively, is then mixed according to different proportion, add hydrochloric acid and ammoniacal liquor as catalyst, prepare silicon phosphorus and be combined wet gel, then prepare composite aerogel through supercritical drying.The composite aerogel obtains Different Pore Structures, the silicon phosphorus composite aerogel of different specific surface areas by adjusting TEOS and TEP different proportion.Preparation method of the present invention is simple, and the silicon phosphorus composite aerogel specific surface area of preparation is more than 700m2/ g, 2.5 μm ~ 25 μm of infrared emittance is more than 0.90.

Description

A kind of high infrared radiance silicon phosphorus composite aerogel and preparation method thereof
Technical field
The present invention relates to aeroge field, and in particular to a kind of high infrared radiance silicon phosphorus composite aerogel and its preparation side Method.
Background technology
Aeroge is a kind of light porous material assembled by nano-scale particle, and solid phase and pore structure are to receive Rice magnitude, porosity may be up to more than 99%, and pore size scope is 1-100nm, wherein more than 80% pore size is less than 50nm.Aeroge has unique performance, such as high-specific surface area, low thermal conductivity and low-k etc., therefore extensively should For photocatalysis carrier（Microporous and Mesoporous Materials, 2004, 75(1):143-147.）, water Handle medium（Journal of Non-Crystalline Solids, 1995, 186(6): 402-407.）, electrical insulator （Journal of Non-Crystalline Solids, 2004, 350(7): 336-344.）In terms of.From 1931 this The S.S.Kistler of Tan Fu universities prepares SiO with waterglass by sol-gel technology and Supercritical Drying Technology first2 Since aeroge, the preparation and application of aeroge obtain great development.The composite aerogel having now been developed at present has As many as tens kinds, including inorganic aerogels (SiO2、Al2O3、TiO2Deng), organic aerogel resorcinol-formaldehyde (RF), Carbamide (MF), Organic-inorganic composite aeroge and carbon aerogels etc..But it is due to the expansion of application field, market Functionalized application to aeroge proposes more requirements, and the species of multi-functional composite aerogel also needs further increase, To meet the market demand.
Meanwhile, with the rise of infrared heating technique, high emissivity, low cost, new infrared radiation easy to use are applied The research of layer material and device is received significant attention.Infrared radiant material high emissivity is that the dipole moment as caused by particle vibration becomes Change what is produced, according to vibration symmetry principle, symmetry during particle vibration is lower, and the change of dipole moment is bigger, and its is infrared Radiation is stronger.So the symmetry of reduction material structure, recurring structure distortion, can effectively lift the hair of infrared radiant material Penetrate performance.Yan Guojin etc. passes through a certain amount of Fe that adulterated into cordierite2O3、MnO2、Ni2O3Deng metal oxide, the iron of preparation Ferrite all band emissivity is 0.87.Fan Xian etc. is with Fe2O3It is primary raw material with cordierite, by adding MnO2With Cr2O3High temp, infrared radiation material is prepared, its emissivity that 6 ~ 20um wave bands are measured under the conditions of 800 DEG C is up to 0.94. Relative to the IR Radiation Ceramic Materials of solid-phase sintering, the composite aerogel tool with nanoscale skeleton structure, high-specific surface area Have the advantages that structural symmetry is low, infrared emission coefficient is high and prepare simple efficient.Element phosphor is introduced silica aerogel by the present invention, Silicon phosphorus composite aerogel is prepared, its microcosmic asymmetry is further reduced, so as to obtain the high property that infrared emittance is more than 0.90 Energy infra-red radiation aeroge, is expected to be applied to high temperature resistant infra-red radiation device of new generation.
The content of the invention
It is an object of the invention to provide a kind of novel, high-specific surface area, it can be applied to the silicon phosphorus of infrared radiating coating Composite aerogel.The present invention prepares silicon phosphorus composite aerogel using esters silicon source and phosphorus source, and preparation technology is simple, and for preparing answers Close aeroge specific surface area big, density is low, can be used for a long time at high temperature, and the introducing of phosphorus can increase composite aerogel Infrared emittance, is expected to be applied to high temperature resistant infrared radiating coating.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel, this method is with tetraethyl orthosilicate and tricresyl phosphate second Ester is raw material, and SiO is prepared by the way of hydrolyzing respectively2Colloidal sol and P2O5Colloidal sol, then by SiO2Colloidal sol and P2O5Colloidal sol mixing system Standby SiO2-P2O5Wet gel, then high infrared radiance silicon phosphorus composite aerogel is prepared by supercritical drying.
It is preferred that, comprise the following steps：
（1）SiO2The preparation of colloidal sol：By tetraethyl orthosilicate (TEOS), ethanol (EtOH) and water (H2O) it is uniformly mixed, then PH value is adjusted to 1 ~ 3, hydrolysis obtains the SiO of clear2Colloidal sol；
（2）P2O5The preparation of colloidal sol：Triethyl phosphate (TEP), second alcohol and water are uniformly mixed, then it is 2 ~ 4 to adjust pH value, Hydrolysis, obtains the P of clear2O5Colloidal sol；
（3）SiO2-P2O5The preparation of compound moisture gel：By SiO2Colloidal sol and P2O5Colloidal sol is mixed, and is then stirred at 25 DEG C ~ 45 DEG C It is 4 ~ 6 that pH value is adjusted after mixing, and obtains SiO2-P2O5Wet gel, then use soaked in absolute ethyl alcohol SiO2-P2O5Wet gel, obtains SiO2- P2O5Compound moisture gel；
（4）Supercritical drying：Step（3）Gained SiO2-P2O5High infrared radiance is made through supercritical drying in compound moisture gel Silicon phosphorus composite aerogel.
It is further preferred that step（1）The tetraethyl orthosilicate, the mol ratio of second alcohol and water are 1:2:4~1:4:8.
It is further preferred that step（1）, step（2）The time of the hydrolysis is 1 ~ 3h.
It is further preferred that step（1）, step（2）The time of the stirring is 15min.
It is further preferred that step（1）, step（2）Adjust the hydrochloric acid that the equal concentration of pH value is 0.01mol/L.
It is further preferred that step（2）The triethyl phosphate, the mol ratio of second alcohol and water are 1:2:4~1:4:8.
It is further preferred that step（3）The SiO2Colloidal sol and P2O5Colloidal sol is 1 by silicon phosphorus mol ratio:1~9:1 mixing.
It is further preferred that step（3）The time of the stirring is 1 ~ 3h.
It is further preferred that step（3）The temperature of the immersion is 25 DEG C ~ 45 DEG C, and the time is 3 ~ 5 days.
It is further preferred that step（3）Adjust the ammoniacal liquor that the equal concentration of pH value is 0.05mol/L.
It is further preferred that step（4）The supercritical drying uses CO2For fluid, drying process is Pc=10MPa, Tc =308.15K ~ 328.15K, drying time is 3 ~ 5h.
A kind of high infrared radiance silicon phosphorus composite aerogel as made from the process described above, the silicon phosphorus composite aerogel It is a kind of non-crystalline solids material, specific surface area is more than 700m2/ g, the infrared emittance of 2.5 μm ~ 25 mu m wavebands is more than 0.90.
Compared with prior art, the present invention has the effect that：
（1）The invention provides a kind of preparation technology of silicon phosphorus composite aerogel, the composite aerogel pore size distribution prepared is uniform, Specific surface area is big, density is low, and these parameters can be adjusted by experiment parameter.
（2）Element phosphor is introduced silica aerogel system by the present invention, further increase material microcosmic asymmetry, and preparation is answered The infrared radiation property for closing aeroge is good (infrared emittance of 2.5 μm ~ 25 mu m wavebands is more than 0.90), and resistance to elevated temperatures is good, has Hope and be applied to high temperature resistant infrared radiation coating.
Brief description of the drawings
Fig. 1 is the TEM photos of the gained silicon phosphorus composite aerogel of embodiment 1.
Fig. 2 is the N of the gained silicon phosphorus composite aerogel of embodiment 12Adsorption/desorption curve figure.
Fig. 3 is the grading curve figure of the gained silicon phosphorus composite aerogel of embodiment 1.
Embodiment
The specific implementation of the present invention is described further with example below in conjunction with the accompanying drawings, but embodiments of the present invention are not It is limited to this, to not specified technological parameter, can refer to routine techniques progress.
Embodiment 1
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed at 25 DEG C, 1.8mL0.1mol/L mixed in hydrochloric acid stirring is added 1h, obtains the SiO of clear2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed and stirred at 25 DEG C, 2.0mL 0.01mol/L mixed in hydrochloric acid is added 1h is stirred, the P of clear is obtained2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 1 according to silicon phosphorus mol ratio:1 mixing, continues at 25 DEG C 1h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 4, obtains SiO2-P2O5Wet gel, with 15mL anhydrous second Alcohol seals immersion SiO at 25 DEG C2-P2O5Wet gel 3 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=308.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 7.1nm, and specific surface area is 787.6m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.932.
SiO obtained by the present embodiment2-P2O5Transmission electron microscope photo, the N of aeroge2Adsorption/desorption curve figure and particle diameter distribution are bent Line chart difference is as shown in Figure 1, Figure 2, Figure 3 shows.SiO obtained by other embodiments2-P2O5Transmission electron microscope photo, the N of aeroge2Absorption Desorption curve figure and grading curve figure are essentially identical with Fig. 1, Fig. 2, Fig. 3 respectively, no longer provide one by one.
Embodiment 2
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed at 35 DEG C, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring is added 1h, obtains the SiO of clear2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed at 35 DEG C, the mixed in hydrochloric acid for adding 2.0mL 0.01mol/L is stirred 1h is mixed, the P of clear is obtained2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 2 according to silicon phosphorus mol ratio:1 mixing, continues at 35 DEG C 2h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 5, obtains SiO2-P2O5Wet gel, with 15mL anhydrous second Alcohol seals immersion SiO at 35 DEG C2-P2O5Wet gel 3 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=318.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 8.0nm, and specific surface area is 849.4m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.946.
Embodiment 3
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed at 45 DEG C, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring is added 1h, obtains the SiO of clear2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed at 45 DEG C, the mixed in hydrochloric acid for adding 2.0mL 0.01mol/L is stirred 1h is mixed, the P of clear is obtained2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 3 according to silicon phosphorus mol ratio:1 mixing, continues at 45 DEG C 3h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 6, obtains SiO2-P2O5Wet gel, with 15mL anhydrous second Alcohol seals immersion SiO at 45 DEG C2-P2O5Wet gel 3 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=328.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 7.7nm, and specific surface area is 857.9m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.954.
Embodiment 4
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed at 25 DEG C, 1.8mL0.1mol/L mixed in hydrochloric acid stirring is added 1h, obtains the SiO of clear2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed and stirred at 25 DEG C, 2.0mL 0.01mol/L mixed in hydrochloric acid is added 1h is stirred, the P of clear is obtained2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 4 according to silicon phosphorus mol ratio:1 mixing, continues at 25 DEG C 1h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 5, obtains SiO2-P2O5Wet gel, with 20mL anhydrous second Alcohol seals immersion SiO at 25 DEG C2-P2O5Wet gel 4 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=328.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 5.9nm, and specific surface area is 746.7m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.907.
Embodiment 5
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring 1h is added, obtains clear Clear bright SiO2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed, 2.0mL 0.01mol/L mixed in hydrochloric acid stirring 1h is added, obtains The P of clear2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 5 according to silicon phosphorus mol ratio:1 mixing, continues at 35 DEG C 2h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 6, obtains SiO2-P2O5Wet gel, with 20mL anhydrous second Alcohol seals immersion SiO at 35 DEG C2-P2O5Wet gel 4 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=308.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 7.9nm, and specific surface area is 813.4m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.920.
Embodiment 6
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring 1h is added, obtains clear Clear bright SiO2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed, 2.0mL 0.01mol/L mixed in hydrochloric acid stirring 1h is added, obtains The P of clear2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 6 according to silicon phosphorus mol ratio:1 mixing, continues at 45 DEG C 3h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 4, obtains SiO2-P2O5Wet gel, with 20mL anhydrous second Alcohol seals immersion SiO at 45 DEG C2-P2O5Wet gel 4 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=318.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 8.1nm, and specific surface area is 856.1m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.926.
Embodiment 7
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed, 1.8mL, 0.1mol/L mixed in hydrochloric acid stirring 1h is added, obtains clear Clear bright SiO2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 23.3mL absolute ethyl alcohol (EtOH) and 3.6mL deionized water (H2O 15min) is mixed and stirred for, 2.0mL 0.01mol/L mixed in hydrochloric acid stirring 1h is added, obtains To the P of clear2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 7 according to silicon phosphorus mol ratio:1 mixing, continues at 25 DEG C 1h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 6, obtains SiO2-P2O5Wet gel, with 25mL anhydrous second Alcohol seals immersion SiO at 25 DEG C2-P2O5Wet gel 5 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=318.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 7.0nm, and specific surface area is 987.0m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.934.
Embodiment 8
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring 1h is added, obtains clear Clear bright SiO2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 34.9mL absolute ethyl alcohol (EtOH) and 5.4mL deionized water (H2O 15min) is mixed, 2.0mL 0.01mol/L mixed in hydrochloric acid stirring 1h is added, obtains The P of clear2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 8 according to silicon phosphorus mol ratio:1 mixing, continues at 35 DEG C 2h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 4, obtains SiO2-P2O5Wet gel, with 25mL anhydrous second Alcohol seals immersion SiO at 35 DEG C2-P2O5Wet gel 5 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=328.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 7.3nm, and specific surface area is 915.8m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.927.
Embodiment 9
A kind of preparation method of high infrared radiance silicon phosphorus composite aerogel：
（1）SiO2The preparation of colloidal sol：By 22.3mL tetraethyl orthosilicate (TEOS), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed, 1.8mL 0.1mol/L mixed in hydrochloric acid stirring 1h is added, obtains clear Clear bright SiO2Colloidal sol.
（2）P2O5The preparation of colloidal sol：By 17mL triethyl phosphate (TEP), 46.5mL absolute ethyl alcohol (EtOH) and 7.2mL deionized water (H2O 15min) is mixed, 2.0mL 0.01mol/L mixed in hydrochloric acid stirring 1h is added, obtains The P of clear2O5Colloidal sol.
（3）The SiO completed will be prepared2Colloidal sol and P2O5Colloidal sol is 9 according to silicon phosphorus mol ratio:1 mixing, continues at 45 DEG C 3h is stirred, 0.05mol/L ammoniacal liquor is then added, regulation pH value is 5, obtains SiO2-P2O5Wet gel, with 25mL anhydrous second Alcohol seals immersion SiO at 45 DEG C2-P2O5Wet gel 5 days, respectively replaces an absolute ethyl alcohol, most afterwards through overcritical titanium dioxide sooner or later Carbon dries 4h (PC = 10 MPa and TC=308.15 K) prepare SiO2-P2O5Aeroge.
Test SiO obtained by the present embodiment2-P2O5The average pore size of aeroge is 8.0nm, and specific surface area is 857.2m2/ g, 2.5 μm ~ 25 μm of infrared emittance is 0.905.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the common skill of art Art personnel should be appreciated that can modify or equivalent substitution with reference to above-described embodiment to the embodiment of the present invention, These any modifications or equivalent substitution without departing from spirit and scope of the invention are applying for that pending claim protects model Within enclosing.

Claims (10)

1. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel, it is characterised in that this method is with tetraethyl orthosilicate And triethyl phosphate is raw material, and SiO is prepared by the way of hydrolyzing respectively2Colloidal sol and P2O5Colloidal sol, then by SiO2Colloidal sol and P2O5 Colloidal sol is mixed with SiO2-P2O5Wet gel, then high infrared radiance silicon phosphorus composite aerogel is prepared by supercritical drying.
2. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 1, it is characterised in that Comprise the following steps：
（1）SiO2The preparation of colloidal sol：Tetraethyl orthosilicate, second alcohol and water are uniformly mixed, then adjust pH value to 1 ~ 3, is hydrolyzed, Obtain the SiO of clear2Colloidal sol；
（2）P2O5The preparation of colloidal sol：Triethyl phosphate, second alcohol and water are uniformly mixed, then it is 2 ~ 4 to adjust pH value, hydrolysis, Obtain the P of clear2O5Colloidal sol；
（3）SiO2-P2O5The preparation of compound moisture gel：By SiO2Colloidal sol and P2O5Colloidal sol is mixed, and is then stirred at 25 DEG C ~ 45 DEG C Mix, then it is 4 ~ 6 to adjust pH value, obtains SiO2-P2O5Wet gel, then use soaked in absolute ethyl alcohol SiO2-P2O5Wet gel, obtains SiO2- P2O5Compound moisture gel；
（4）Supercritical drying：Step（3）Gained SiO2-P2O5High infrared radiance is made through supercritical drying in compound moisture gel Silicon phosphorus composite aerogel.
3. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（1）The tetraethyl orthosilicate, the mol ratio of second alcohol and water are 1:2:4~1:4:8.
4. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（1）, step（2）The time of the hydrolysis is 1 ~ 3h.
5. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（2）The triethyl phosphate, the mol ratio of second alcohol and water are 1:2:4~1:4:8.
6. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（3）The SiO2Colloidal sol and P2O5Colloidal sol is 1 by silicon phosphorus mol ratio:1~9:1 mixing.
7. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（3）The time of the stirring is 1 ~ 3h.
8. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（3）The temperature of the immersion is 25 DEG C ~ 45 DEG C, and the time is 3 ~ 5 days.
9. a kind of preparation method of high infrared radiance silicon phosphorus composite aerogel according to claim 2, it is characterised in that Step（4）The supercritical drying uses CO2For fluid, drying process is Pc=10MPa, Tc=308.15K ~ 328.15K, is dried Time is 3 ~ 5h.
10. a kind of high infrared radiance silicon phosphorus composite aerogel as made from the method described in claim any one of 1-9, it is special Levy and be, the specific surface area of the silicon phosphorus composite aerogel is more than 700m2/ g, the infrared emittance of 2.5 μm ~ 25 mu m wavebands is more than 0.90。
CN201710498161.1A 2017-06-27 2017-06-27 A kind of high infrared radiance silicon phosphorus composite aerogel and preparation method thereof Pending CN107324348A (en)

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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
CN101445356A (en) * 2008-11-27 2009-06-03 中南大学 Nano-hole aerogel heat-insulating composite material and preparation method thereof
CN101628804A (en) * 2008-07-18 2010-01-20 山东鲁阳股份有限公司 Aerogel heat insulation composite material and preparation method thereof
CN102584010A (en) * 2012-03-15 2012-07-18 河南工业大学 Preparation method of multi-component aerogel
CN106431186A (en) * 2016-09-05 2017-02-22 北京工业大学 Method for preparing fiber-loaded rutile type TiO2 composite SiO2 aerogel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101628804A (en) * 2008-07-18 2010-01-20 山东鲁阳股份有限公司 Aerogel heat insulation composite material and preparation method thereof
CN101445356A (en) * 2008-11-27 2009-06-03 中南大学 Nano-hole aerogel heat-insulating composite material and preparation method thereof
CN102584010A (en) * 2012-03-15 2012-07-18 河南工业大学 Preparation method of multi-component aerogel
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Application publication date: 20171107