CN109721322A - Modification infusorial earth-silicon dioxide silica aerogel composite material and its preparation method and application - Google Patents
Modification infusorial earth-silicon dioxide silica aerogel composite material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of modification infusorial earth-silicon dioxide silica aerogel composite materials and its preparation method and application, the composite material is prepared by the following method: step 1, diatomite pretreatment: diatomite is placed in aqueous hydrochloric acid solution and is sufficiently stirred, filters, wash and dry；Step 2, modification infusorial earth is placed in deionized water and is stirred by ultrasonic, form it into diatomite turbid；Ethyl orthosilicate, dehydrated alcohol, KH570 and hydrochloric acid are stirred evenly to form reaction system, finally by the diatomite turbid and the reaction system mixed hydrolysis, aging；Step 3, the gel after aging is placed in HMDZ/ n-hexane mixed solution and carries out silicic acid anhydride, be destroyed during constant pressure and dry with the pore structure of anti-gel；Step 4, under normal pressure, sample will be placed in dry 1-4h in 60-100 DEG C of environment obtained by step 3.Composite material compressive property of the invention is strong, and heat-proof quality is good.
Description
Technical field
The present invention relates to aerogel composite technical fields, more particularly to a kind of modification infusorial earth-silica gas
Gel complex material and its preparation method and application.
Background technique
SiO2Aeroge is a kind of amorphous material of nano aperture, has low density, large specific surface area, porosity height etc.
Feature.And its unique nanoporous reticular structure can greatly limit the gentle phase thermal convection of solid phase heat transfer, have excellent
Different thermal and insulating performance, so having greatly development prospect in building thermal insulation material.But then, SiO2Airsetting
This structure of glue also determines the major defect that its own intensity is low, brittleness is big, to make it difficult to by as a kind of efficient
Heat-barrier material and directly apply in building thermal insulation material.
In recent years, scientists are more deep to the research of aerogel composite.Up to the present, there are many
Aerogel composite is prepared out, but often all there is certain performance deficiencies.Such as Kim etc. is with polyethylene particle
Polyethylene/the SiO with certain mechanical strength is prepared for for reinforced phase2Aerogel composite, but its thermal coefficient is higher
(can reach 0.12W/mk)；And Deng etc. is then by being added ceramic fibre come to SiO2Aeroge progress is compound, resulting
Although composite material is promoted in mechanical property, it is still only 0.128MPa.That is, it is difficult to obtain while having
The SiO of good heat-proof quality and mechanical property2Aerogel composite.
Diatomite has many advantages, such as small density, large specific surface area, from a wealth of sources, cheap, it is often more important that, it can be with
The mechanical performance of material is improved as reinforced phase.One kind solving the modification diatom of problem above using diatomite as reinforced phase
Soil-silicon dioxide silica aerogel composite material and preparation method thereof needs further to research and develop.
Summary of the invention
In view of the technical drawbacks of the prior art, it is an object of the present invention to provide a kind of modification infusorial earth-dioxies
SiClx aerogel composite and preparation method thereof, the present invention are reinforced phase and SiO by coupling agent, diatomite of KH5702It is molten
Glue is mixed, and after gel, hydrophobization, ageing process, is prepared for modification infusorial earth/SiO by constant pressure and dry2Aeroge
Composite material, and the influence with regard to different diatomite dosages to thermal conductivity of composite materials, porosity and compression strength carries out
Analysis.
The technical solution adopted to achieve the purpose of the present invention is:
A kind of modification infusorial earth-silicon dioxide silica aerogel composite material, the thermal coefficient of the composite material is 0.03~
0.04W/mk, average pore size are 9~17nm, and specific surface area is 600~850m2/ g, compressive strength 0.4-0.6Mpa；
The composite material is prepared in accordance with the following methods:
Step 1, diatomite pre-processes:
Diatomite is placed in aqueous hydrochloric acid solution and is sufficiently stirred, to remove the mineralogical composition in diatomite, filters, wash simultaneously
Drying obtains modification infusorial earth；
Step 2, modification infusorial earth is placed in deionized water and is stirred by ultrasonic, form it into diatomite turbid；By positive silicic acid
Ethyl ester, dehydrated alcohol, KH570 and hydrochloric acid stir evenly to form reaction system, wherein ethyl orthosilicate, dehydrated alcohol, KH570
Molar ratio with hydrogen chloride in hydrochloric acid is (20-30): (150-200): (1.5-2.5): (0.5-1.5)；Finally by the diatom
Native turbid and the reaction system mixed hydrolysis, wherein the quality of modification infusorial earth is the 5wt%- of silicon source TEOS mass
Weak aqua ammonia is added after 25wt%, 20-50min and obtains wet gel, the wet gel is immersed in the mixed liquor of dehydrated alcohol and water
Middle carry out aging, wherein the volume ratio of dehydrated alcohol and water is (5-10): 1, it carries out two to four times altogether, each 10-15h；
Step 3, the gel after aging is placed in HMDZ (hexamethyldisilazane)/n-hexane mixed solution carry out it is hydrophobic
Change processing, is destroyed during constant pressure and dry with the pore structure of anti-gel, and wherein the volume ratio of HMDZ/ n-hexane is (1-
2): (10-20)；
Step 4, under normal pressure, sample is placed in 60-100 DEG C of environment by step 3 gained and dries 1-4h to get modified silicon
Diatomaceous earth/SiO2Aerogel composite.
Preferably, in the step 2 modification infusorial earth quality be silicon source TEOS mass 10wt%-20wt%, preferably
For 15wt%.
Preferably, the thermal coefficient of the composite material is 0.032~0.036W/mk, and average pore size is 10~12nm, than
Surface area is 700~800m2/ g, compressive strength 0.51-0.55Mpa.
Another aspect of the present invention further includes a kind of preparation side of modification infusorial earth-silicon dioxide silica aerogel composite material
Method, comprising the following steps:
Step 1, diatomite pre-processes:
Diatomite is placed in aqueous hydrochloric acid solution and is sufficiently stirred, to remove the mineralogical composition in diatomite, filters, wash simultaneously
Drying obtains modification infusorial earth；
Step 2, modification infusorial earth is placed in deionized water and is stirred by ultrasonic, form it into diatomite turbid；By positive silicic acid
Ethyl ester, dehydrated alcohol, KH570 and hydrochloric acid stir evenly to form reaction system, wherein ethyl orthosilicate, dehydrated alcohol, KH570
Molar ratio with hydrogen chloride in hydrochloric acid is (20-30): (150-200): (1.5-2.5): (0.5-1.5)；Finally by the diatom
Native turbid and the reaction system mixed hydrolysis, wherein the quality of modification infusorial earth is the 5wt%- of silicon source TEOS mass
Weak aqua ammonia is added after 25wt%, 20-50min and obtains wet gel, the wet gel is immersed in the mixed liquor of dehydrated alcohol and water
Middle carry out aging, wherein the volume ratio of dehydrated alcohol and water is (5-10): 1, it carries out two to four times altogether, each 10-15h；
Step 3, the gel after aging is placed in HMDZ (hexamethyldisilazane)/n-hexane mixed solution carry out it is hydrophobic
Change processing, is destroyed during constant pressure and dry with the pore structure of anti-gel, and wherein the volume ratio of HMDZ/ n-hexane is (1-
2): (10-20)；
Step 4, under normal pressure, sample is placed in 60-100 DEG C of environment by step 3 gained and dries 1-4h to get modified silicon
Diatomaceous earth/SiO2Aerogel composite.
Preferably, in the step 3 modification infusorial earth quality be silicon source TEOS mass 10wt%-20wt%, preferably
For 15wt%.
Another aspect of the present invention further includes that the modification infusorial earth-silicon dioxide silica aerogel composite material is protected in building
Application in adiabator.
Preferably, the thermal coefficient of the composite material is 0.032~0.036W/mk, and average pore size is 10~12nm, than
Surface area is 700~800m2/ g, compressive strength 0.51-0.55Mpa.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention is reinforced phase by silicon source, diatomite of ethyl orthosilicate, using sol-gel and constant pressure and dry technique
It is prepared for diatomite/SiO2Aerogel composite, process is simple, easy to promote and utilize.
2, intensity is high, good heat-insulation effect, is suitable for building thermal insulation material use.
Detailed description of the invention
Fig. 1 (a)-(b) show respectively composite diatomite aeroge (15wt% diatomite) under different amplification
SEM picture.
The N2 adsorption desorption curve of Fig. 2 (a) difference diatomite content aerogel composite.
(b) graph of pore diameter distribution of different diatomite content aerogel composites.
Fig. 3 is the thermal coefficient of different diatomite content aerogel composites.
The average compressive strength of Fig. 4 difference diatomite content aerogel composite.
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.It should be appreciated that described herein
Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
The experimental material and equipment of following embodiment are as follows:
Vinyltriethoxysilane (KH570): analysis is pure, and Nanjing is through Tian Wei Chemical Co., Ltd.；Two silicon nitrogen of hexamethyl
Alkane (HMDZ): pure, Shaoxing Shangyu Hua Lun Chemical Co., Ltd. is analyzed；Ethyl orthosilicate (TEOS): analysis is pure, Tianjin recovery
Fine Chemical Co., Ltd；Dehydrated alcohol (ETOH): pure, Tianjin Jin Dong Tian Zheng fine chemistry chemical reagent work is analyzed；N-hexane:
Analyze pure, Tianjin Jin Dong Tian Zheng fine chemistry chemical reagent work；Ammonium hydroxide: pure, Tianjin benchmark chemical reagent Co., Ltd is analyzed；Salt
Acid: pure, section's prestige (Tianjin) Chemical Co., Ltd. is analyzed；Diatomite: extremely big filter aid factory.
DF-101S type heat collecting type constant-temperature heating magnetic stirring apparatus, Yuhua Instrument Co., Ltd., Gongyi City；JJ-1 is accurate
Timing electric mixer, high honour instrument manufacturing Co., Ltd, Jintan City；S-4800 scanning electron microscope (SEM), Hitachi, Japan
Company；3H-2000PSI type specific surface area and Porosimetry, scientific and technological (Beijing) Co., Ltd of Bei Shide instrument.
The present embodiment modification infusorial earth-silicon dioxide silica aerogel composite material preparation process, comprising the following steps:
Step 1, diatomite pre-processes:
Effectively to remove the mineralogical composition in diatomite, diatomite is placed in a beaker to and is added appropriate hydrochloric acid and water (acid
Water is than being about 5:1), it filtered, washed and is dried after electromagnetic agitation 3h, obtain modification infusorial earth.
Step 2, the modification infusorial earth that a certain amount of step 1 obtains is weighed with beaker, add suitable deionized water and surpassed
Sound stirs 15 minutes, forms it into diatomite turbid；
The ethyl orthosilicate of certain mol proportion, dehydrated alcohol, KH570 and a small amount of hydrochloric acid are stirred evenly and are placed on round mouth burning
Reaction system is obtained in bottle；
Finally the diatomite turbid and the reaction system are mixed and start to hydrolyze, a small amount of dilute ammonia is added after 30min
Water obtain gel simultaneously carry out aging, wherein the quality of modification infusorial earth be respectively silicon source TEOS mass 5wt%, 10wt%,
15wt%, 20wt%, 25wt%；
Gel after aging is placed in configured HMDZ/ n-hexane mixed solution by a certain percentage and is carried out at hydrophobization
Reason, is destroyed during constant pressure and dry with the pore structure of anti-gel.Sample is finally respectively placed in 60,80,100 DEG C
Dry 2h is in environment to get diatomite/SiO2Aeroge composite reinforcing material.
This experiment using the dosage of modification infusorial earth as variable, be utilized respectively 5wt%, 10wt% by silicon source TEOS dosage,
15wt%, 20wt%, 25wt% carry out sample preparation, at the same with pure SiO2Aeroge is compared.Using SEM, nitrogen
Adsorption/desorption, thermal coefficient and compressive strength to gained sample are characterized and are analyzed.
By taking 15wt% diatom soil sample as an example, using scanning electron microscope to diatomite/SiO2Aerogel composite it is microcosmic
Morphology analysis, as shown in Figure 1.
Prepare diatomite/SiO2The key of aerogel composite is the combination problem between two-phase.Work as SiO2Colloidal sol immerses
To after the gap between diatomite particle, entire compound system can be strutted, to realize being uniformly distributed for diatomite particle.And
And it is modified by KH570, the great amount of hydroxy group on diatomite particle and silica-based aerogel surface can be by dredging containing unsaturation C=C
Replaced water alkyl, so that the combination on chemical bond level can be realized by certain addition reaction between the two.
Fig. 1 (a), (b) are respectively diatomite/SiO2Aerogel composite (15wt%) is under different amplification
SEM image.From Fig. 1 (a) as can be seen that sample is after constant pressure and dry, most of gap between diatomite particle is by bulk
Aeroge is filled；Such as Fig. 1 (b) after being amplified to diatomite particle, it can clearly be seen that having on the surface of its relative smooth
Many is distributed by the porous network structure that nano-scale particle forms, and shows diatomite particle and SiO2Aeroge realizes ratio
More uniform mixing.
Each sample is detected by 3H-2000PSI type specific surface area and Porosimetry, acquired results such as Fig. 2
(a), shown in (b) and table 1.
The specific surface area and pore-size distribution of 1 each sample of table
Fig. 2 (a), (b) are respectively N2 adsorption desorption curve and pore-size distribution of the composite material under different diatomite contents
Figure；Table 1 is then corresponding specific surface area and average aperture value.By Fig. 2 (a) it is found that N2With the adsorption desorption curve of material
For IV type, belong to the scope of mesoporous material；Adsorption-desorption curve is all in about p/p0It is separated when=0.6, explanation
With the presence of central hole structure；With the rising of diatomite content, the hysteresis loop of curve is gradually decreased, in conjunction with table 1 it is found that the phenomenon
Caused by being mainly gradually reduced due to the specific surface area of composite material.
It can be obtained by Fig. 2 (b), when diatomite additional amount gradually increases, pore size distribution range is first to increase to tend to be steady afterwards
(using 15wt% as boundary's point).When diatomite content is less, part SiO2Aerogel particle can be attached to diatomite inner hole wall
In cause its aperture to be obviously reduced, but with the increase of diatomite content, this attachment phenomenon of aeroge can be more unknown
It is aobvious, so that the pore-size distribution of composite material is gradually increased and tends to be saturated.But in conjunction with table 1, the pore-size distribution of composite material
Although average pore size is to be gradually reduced being gradually increased, reason may be since the addition of bulky grain diatomite hinders
The progress of gel hydrophobization process is hindered, so that occurring what pore structure excess shrinkage in part was even destroyed in the drying process
Phenomenon.
Sample merging Conduction Coefficient Detector Basing after grinding is tested, acquired results are as shown in Figure 3.Pure aerogel material
Thermal coefficient has increased to 0.0302W/mk by 0.0202W/mk after diatomite is added, at the same time, diatomite/SiO2Airsetting
The thermal conductivity of glue composite material increases and slowly rises also with diatomite dosage.Concrete reason is as follows:
The heat transfer mechanism of material mainly includes three parts: heat transfer, thermal convection and heat radiation.Usually in room temperature, material
The conduction heat transfer of material is negligible.And under thermal equilibrium state, the spectral radiant exitance of radiator and its spectral absorption
The ratio of ratio is then the function of radiation wavelength and temperature, unrelated with radiator nature (Kirchhoff's law of radiation), i.e.,
The heat radiation conduction numerical value of material can regard a constant as.At the same time, for general nanoporous SiO2Aeroge and
Speech, up to 95% porosity make its solid phase heat transfer and gas phase heat transfer numerical value also not be extremely to protrude.So knot
The conclusion that Fig. 2 is obtained is closed, excess shrinkage occurs for the part pore structure that the addition of large scale diatomite will cause composite material very
To destruction, so that the heat transfer numerical value of material increases rapidly, and integral heat-insulation property variation is eventually led to.
Since common aerogel material intensity is extremely low, so we using diatomite as reinforced phase, silica-based aerogel is base
Body is prepared for diatomite/SiO in conjunction with sol-gel method and constant pressure and dry preparation process2Aerogel composite, and pass through
Average compressive strength is measured to characterize to sample, to probe into influence of the addition of diatomite to aerogel material intensity.It is real
It is as shown in Figure 4 to test result: the compressive strength that the addition of diatomite can greatly improve composite material (is increased to by 0.054MPa
0.458MPa), gradually increasing but with diatomite content, the average compressive strength of material entirety are but rendered as slowly rising
Situation.And excessive diatomite is easy to cause the thermal conductivity of composite material higher, and heat-proof quality is caused to decline.In conjunction with before
Detection, optimal diatomite additional amount should be 15wt% or so.
In conclusion being reinforced phase by silicon source, diatomite of ethyl orthosilicate, using sol-gel and constant pressure and dry work
Skill is prepared for diatomite/SiO2 aerogel composite.To the test result of its heating conduction, pore structure and mechanical property
Show:
(1) diatomite/SiO2 aerogel composite has preferable heat-proof quality, and thermal coefficient range is
0.0312~0.0345W/mk is not much different with the 0.0241W/mk of pure SiO2 aeroge.
(2) average pore size of composite material is between 9.87~16.98nm, specific surface area then 610.3586~
550.4721m2Between/g, illustrate that composite material belongs to nano-porous materials scope.
(3) in terms of compressive strength, composite material can reach 0.551MPa, much higher than pure aeroge
0.054MPa, in conjunction with conclusion (1) it follows that when the incorporation of diatomite reaches 15wt%, resulting composite material is not only
The relatively low thermal coefficient of aeroge itself is remained, while can also greatly improve SiO2The compression strength of aeroge.
The above is only a preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, various improvements and modifications may be made without departing from the principle of the present invention, these are improved and profit
Decorations also should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of modification infusorial earth-silicon dioxide silica aerogel composite material, which is characterized in that the thermal coefficient of the composite material
For 0.03~0.04W/mk, average pore size is 9~17nm, and specific surface area is 600~850m2/ g, compressive strength 0.4-
0.6Mpa；
The composite material is prepared in accordance with the following methods:
Step 1, diatomite pre-processes:
Diatomite is placed in aqueous hydrochloric acid solution and is sufficiently stirred, removing the mineralogical composition in diatomite, filtering, wash and drying
Obtain modification infusorial earth；
Step 2, modification infusorial earth is placed in deionized water and is stirred by ultrasonic, form it into diatomite turbid；By ethyl orthosilicate,
Dehydrated alcohol, KH570 and hydrochloric acid stir evenly to form reaction system, wherein ethyl orthosilicate, dehydrated alcohol, KH570 and hydrochloric acid
The molar ratio of middle hydrogen chloride is (20-30): (150-200): (1.5-2.5): (0.5-1.5)；Finally by the diatomite turbid
With the reaction system mixed hydrolysis, wherein the quality of modification infusorial earth is the 5wt%-25wt%, 20- of silicon source TEOS mass
Weak aqua ammonia is added after 50min and obtains wet gel, the wet gel is immersed in the mixed liquor of dehydrated alcohol and water and carries out aging,
Wherein the volume ratio of dehydrated alcohol and water is (5-10): 1, aging carries out two to four times altogether, each 10-15h；
Step 3, the gel after aging is placed in HMDZ (hexamethyldisilazane)/n-hexane mixed solution and is carried out at hydrophobization
Reason, is destroyed during constant pressure and dry with the pore structure of anti-gel, and wherein the volume ratio of HMDZ/ n-hexane is (1-2):
(10-20)；
Step 4, under normal pressure, sample is placed in 60-100 DEG C of environment by step 3 gained and dries 1-4h to get modified diatom
Soil/SiO2Aerogel composite.
2. a kind of modification infusorial earth-silicon dioxide silica aerogel composite material as described in claim 1, which is characterized in that described
The quality of modification infusorial earth is the 10wt%-20wt%, preferably 15wt% of silicon source TEOS mass in step 2.
3. a kind of modification infusorial earth-silicon dioxide silica aerogel composite material as described in claim 1, which is characterized in that described
The thermal coefficient of composite material is 0.032~0.036W/mk, and average pore size is 10~12nm, and specific surface area is 700~800m2/
G, compressive strength 0.51-0.55Mpa.
4. a kind of preparation method of modification infusorial earth-silicon dioxide silica aerogel composite material, which is characterized in that including following step
It is rapid:
Step 1, diatomite pre-processes:
Diatomite is placed in aqueous hydrochloric acid solution and is sufficiently stirred, removing the mineralogical composition in diatomite, filtering, wash and drying
Obtain modification infusorial earth；
Step 2, modification infusorial earth is placed in deionized water and is stirred by ultrasonic, form it into diatomite turbid；By ethyl orthosilicate,
Dehydrated alcohol, KH570 and hydrochloric acid stir evenly to form reaction system, wherein ethyl orthosilicate, dehydrated alcohol, KH570 and hydrochloric acid
The molar ratio of middle hydrogen chloride is (20-30): (150-200): (1.5-2.5): (0.5-1.5)；Finally by the diatomite turbid
With the reaction system mixed hydrolysis, wherein the quality of modification infusorial earth is the 5wt%-25wt%, 20- of silicon source TEOS mass
Weak aqua ammonia is added after 50min and obtains wet gel, the wet gel is immersed in the mixed liquor of dehydrated alcohol and water and carries out aging,
Wherein the volume ratio of dehydrated alcohol and water is (5-10): 1, it carries out two to four times altogether, each 10-15h；
Step 3, the gel after aging is placed in HMDZ (hexamethyldisilazane)/n-hexane mixed solution and is carried out at hydrophobization
Reason, is destroyed during constant pressure and dry with the pore structure of anti-gel, and wherein the volume ratio of HMDZ/ n-hexane is (1-2):
(10-20)；
Step 4, under normal pressure, sample is placed in 60-100 DEG C of environment by step 3 gained and dries 1-4h to get modified diatom
Soil/SiO2Aerogel composite.
5. a kind of preparation method of modification infusorial earth-silicon dioxide silica aerogel composite material as claimed in claim 4, feature
It is, the quality of modification infusorial earth is the 10wt%-20wt%, preferably 15wt% of silicon source TEOS mass in the step 3.
6. modification infusorial earth-silicon dioxide silica aerogel composite material answering in building thermal insulation material as described in claim 1
With.
7. modification infusorial earth-silicon dioxide silica aerogel composite material answering in building thermal insulation material as claimed in claim 6
With, which is characterized in that the thermal coefficient of the composite material is 0.032~0.036W/mk, and average pore size is 10~12nm, than
Surface area is 700~800m2/ g, compressive strength 0.51-0.55Mpa.
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| CN111439824A (en) * | 2020-03-06 | 2020-07-24 | 浙江正洁环境科技有限公司 | Water treatment biofilm carrier with bacteria promoting performance and preparation method and application thereof |
| CN114436623A (en) * | 2020-11-03 | 2022-05-06 | 李涛 | Inorganic aerogel composite material and preparation method thereof |
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| CN111439824A (en) * | 2020-03-06 | 2020-07-24 | 浙江正洁环境科技有限公司 | Water treatment biofilm carrier with bacteria promoting performance and preparation method and application thereof |
| CN111439824B (en) * | 2020-03-06 | 2022-08-09 | 浙江正洁环境科技有限公司 | Water treatment biofilm carrier with bacteria promoting performance and preparation method and application thereof |
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