CN109133070A - A method of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass - Google Patents

A method of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Download PDF

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CN109133070A
CN109133070A CN201810989421.XA CN201810989421A CN109133070A CN 109133070 A CN109133070 A CN 109133070A CN 201810989421 A CN201810989421 A CN 201810989421A CN 109133070 A CN109133070 A CN 109133070A
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hydrophobic silica
silica aerogel
raw material
supper
waterglass
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王建国
宋鑫
包志康
杨骏
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • C01B33/141—Preparation of hydrosols or aqueous dispersions
    • C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
    • C01B33/143—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/11—Powder tap density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a kind of methods for preparing hydrophobic silica aerogel as the supper-fast normal pressure of raw material using waterglass,, the following steps are included: 1) mixing waterglass with water, instillation aqueous hydrochloric acid solution adjusts pH value, stirring for it, dehydrated alcohol is added to continue to stir, obtains mixture；2) it is added dropwise to dilute ammonia solution in the mixture of step 1) and adjusts pH value, after sol liquid gradually solidifies, aging is carried out under water-bath, forms blocky gel；3) the blocky gel of step 2 is pulverized, is successively filtered after deionized water and dehydrated alcohol washing, filter residue, which immerses in modification liquid, to be stirred, and modified mixed liquor is obtained；4) it by the modification mixed liquor stratification of step 3), takes upper liquid to be immersed in n-hexane and is filtered after agitator treating, filter residue constant pressure and dry obtains the hydrophobic silica aerogel.For the present invention using cheap waterglass as raw material, gained aerosil has the integrality of three-dimensional net structure, greatly shortens the preparation time of aerosil.

Description

It is a kind of to prepare hydrophobic silica aerogel by the supper-fast normal pressure of raw material of waterglass Method
Technical field
The invention belongs to technical field of inorganic material, and in particular to a kind of prepared using waterglass as the supper-fast normal pressure of raw material is dredged The method of water aerosil.
Background technique
Aeroge is mutually coalesced a kind of solid nano porosity with tridimensional network formed by nanoparticle Material, it is to be used the liquid in its hole on the basis of keeping its hole and space net structure not to be destroyed by wet gel Resulting product after air replaces.Aeroge is current world's upper density and the smallest solid material of thermal conductivity.
Fast development of the aeroge industry in the past few decades, nowadays the preparation of most of aerosils is with silicon Alkoxide is as presoma.The most common silicon alkoxide is methyl orthosilicate and ethyl orthosilicate, passes through the hydrolysis and polycondensation of silicon alkoxide Nanoparticle crosslinking is set to get up to form tridimensional network；The drying mode of aeroge be also aeroge preparation important step it One, the current most common drying mode is supercritical drying, and supercritical drying is that one kind goes dehumidifying solidifying in a manner of accurately controlling The method of liquid in glue.But using silicon alkoxide as presoma, the price is very expensive, this is to result in current aeroge industry Not universal enough one of reason；Equally, using the dry wet gel of the method for supercritical drying, there is also safety for supercritical drying The disadvantages of coefficient is low, condition is harsh limits the industrialization and large-scale application of aerogel material, with going out for constant pressure and dry Existing, more and more people start to prepare aeroge with atmosphere pressure desiccation, but the method for constant pressure and dry needs prolonged solvent to hand over Process is changed, treatment process needs differ for 3 days to 15 days, the large-scale production also largely restricted.
Summary of the invention
For above-mentioned technical problem of the existing technology, the purpose of the present invention is to provide one kind using waterglass as raw material The method that supper-fast normal pressure prepares hydrophobic silica aerogel, the present invention is using cheap waterglass as raw material, in dredging for preparation Under the premise of the better performances of water aerosil, when greatly shortening the preparation of the hydrophobic silica aerogel Between.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature Be the following steps are included:
1) water glass solution is mixed with water, being slowly added dropwise into aqueous hydrochloric acid solution to pH value is 2 ~ 4, then pours into beaker together In, it is stirred to form silica solution, dehydrated alcohol is added, continues to stir, obtains mixture；
2) being slowly added dropwise in the mixture of step 1) and being adjusted to pH value into dilute ammonia solution is 7 ~ 8.5, is stood to sol liquid gradually After solidification, the beaker is placed in 40 ~ 50 DEG C of water-bath, heats 20 ~ 40min, carry out aging, formed in beaker blocky solidifying Glue；
3) the blocky gel obtained after step 2 aging is pulverized, 1 ~ 2h of deionized water agitator treating is added, is filtered, filter residue It immersing 0.5 ~ 1.5h of stirring in dehydrated alcohol and carries out exchange of solvent, then filtered, filter residue, which immerses, stirs 0.5 ~ 1h in modification liquid, Mixed liquor must be modified；
4) by the modification mixed liquor stratification of step 3), upper liquid is taken to be immersed in n-hexane after 20 ~ 40min of agitator treating, It is filtered, filter residue constant pressure and dry obtains the hydrophobic silica aerogel.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 1), the volume ratio that water glass solution is mixed with water is 1:1 ~ 2.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature Be in step 1), the volume ratio of silica solution and dehydrated alcohol is 1:1 ~ 5, be added in the silica solution absolute ethyl alcohol and stirring 5 ~ 15min。
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 1), the concentration of aqueous hydrochloric acid solution is 1.5 ~ 2.5mol/L, preferably 2mol/L；The dropwise addition of the aqueous hydrochloric acid solution Speed is 2 drops/s.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 2, the concentration of dilute ammonia solution is 0.2 ~ 0.6mol/L；The rate of addition of the dilute ammonia solution is 2 drops/s.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 3), the quality of the blocky gel after pulverizing and the volume ratio of deionized water are 1:1 ~ 2, and wherein the unit of quality is G, volume unit mL.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature Be in step 3) that filter residue immerses in dehydrated alcohol when stirring, the ratio of the volume of the quality and dehydrated alcohol of filter residue be 1:0.7 ~ 1.5, wherein the unit of quality is g, volume unit mL.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 3), modification liquid is the mixed liquor being made of n-hexane and trim,ethylchlorosilane；In the modification liquid, n-hexane with The volume ratio of trim,ethylchlorosilane is 8 ~ 12:1, preferably 10:1；When being stirred in the filter residue immersion modification liquid, the quality of filter residue Ratio with the volume of modification liquid is 1:1 ~ 2, and wherein the unit of quality is g, volume unit mL.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature It is in step 4), the volume ratio of upper liquid and n-hexane is 1:0.5 ~ 1.5.
A kind of method that hydrophobic silica aerogel is prepared as the supper-fast normal pressure of raw material using waterglass, feature Be hydrophobic silica aerogel made from step 4) tap density be 0.149 ~ 0.164g/cm3, porosity be 93 ~ 94%, average pore size is 20-30 nm.
Compared with the existing technology, what the present invention obtained has the beneficial effect that:
1) present invention prepares hydrophobic aerosil, in guaranty using this cheap material of waterglass as raw material While matter, the expensive cost generated using organic silicon source is greatly reduced, there is very high practical value；
2) hydrophobic silica aerogel produced by the present invention by aging, surface is modified, exchange of solvent, protect solidifying The integrality of glue three-dimensional net structure, while reducing the (trimethyl in modification liquid of existing surface tension of liquid when constant pressure and dry Chlorosilane, which contains the hydrophobic groupings such as a large amount of methyl, may be coupled to molecular skeleton surface, have repulsion to make nonpolar hydrone With preventing when dry due to surface tension of liquid and bring duct the problem of collapsing), substantially reduce drying time；
3) hydrophobic silica aerogel prepared by the present invention, by gel crush, by inorganic ions wash and etc. (by going Ionized water washs inorganic salts remaining in gel duct, so that in surface hydrophobicity modification procedure, hydrophobic grouping energy Channel surfaces are connected to well, in the drying process, moisture can preferably volatilize product, and gel keeps preferable hole Road；), time needed for greatly reducing entire preparation flow, whole preparation process can be reduced within 8 hours, relative to The prior art greatly shortens the preparation time of hydrophobic silica aerogel, has great reality for large-scale production Meaning；
4) the present invention provides a kind of using industrial waterglass as the supper-fast method for preparing hydrophobic silica aerogel of raw material, packet It includes: ethyl alcohol being added into silica solution obtained, promote gel；The gel pulverized, which immerses in deionized water, to be followed by stirring and washing, with Inorganic salts in gel duct are washed；Gel after deionized water is washed, then solvent friendship is carried out through dehydrated alcohol It changes, water coke slurry most of in duct is come out, the surface tension of solvent is reduced in the drying process, table then is carried out to gel Face is modified, and gel surface is made to become hydrophobicity from hydrophily, can be supper-fast prepare cheap hydrophobic silica airsetting Glue；
5) hydrophobic silica aerogel preparation condition provided by the invention is mild, not high to equipment requirement, and daily energy consumption is smaller, The entire process used time is short, improves production efficiency, reduces cost, is easy to industrialize.
Detailed description of the invention
Fig. 1 is implementing process flow chart of the present invention；
Fig. 2 is the SEM figure of hydrophobic silica aerogel obtained in the embodiment of the present invention 1；
Fig. 3 is the FTIR figure of hydrophobic silica aerogel made from present example 1.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the scope of protection of the present invention is not limited thereto.
In following example 1 ~ 4 and comparative example 1 ~ 2:
It is mixed liquor that 10:1 is formed that modification liquid is by n-hexane and trim,ethylchlorosilane by volume；Industrial-grade sodium silicate solution Mass concentration be 25%-27%(water glass solution be sodium silicate aqueous solution)；The unit of quality is g, and the unit of volume is mL.
Embodiment 1:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) after 1:1 is mixed by volume, instilling concentration by 2 drops/s speed is 1.5mol/L's for industrial-grade sodium silicate solution and water It is 2 that aqueous hydrochloric acid solution, which is adjusted to pH value, then pours into beaker together, is stirred to form silica solution, in silica solution by volume Dehydrated alcohol, which is added, in 1:1 continues to stir 5min, obtains mixture；
2) in the mixture of step 1), being slowly added dropwise into concentration is that be adjusted to pH value be 7(rate of addition to 0.2mol/L dilute ammonia solution It for 2 drops/s), stands after sol liquid in beaker gradually solidifies, the beaker is placed in 40 DEG C of water-bath, heat 20min, Aging is carried out, forms blocky gel in beaker；
3) the blocky gel obtained after step 2 aging is pulverized, the deionized water (quality and deionized water of blocky gel is added Volume ratio 1:1), 1h is followed by stirring and washing, filter, filter residue immerse dehydrated alcohol in stirring 0.5h carry out exchange of solvent after (its The ratio of the quality of middle filter residue and the volume of the dehydrated alcohol is 1:0.7), then filtered, filter residue, which immerses in modification liquid, to be stirred 1h(filter residue immerses in modification liquid, and the ratio of the volume of the quality of the filter residue and the modification liquid is 1:1), obtain modified mixed liquor；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, by volume 1: 0.5 to be immersed in agitator treating 20min(i.e. upper liquid and the volume ratio of n-hexane in n-hexane be 1:0.5), it is filtered, filter residue The constant pressure and dry 1h at 60 DEG C, obtains the hydrophobic silica aerogel.
It is scanned electron microscope (SEM) to hydrophobic silica aerogel made from the present embodiment to be analyzed and characterized, knot Fruit is as shown in Figure 2；From figure 2 it can be seen that the aeroge is formed by connecting by many nanoscale particles, particle diameter distribution is more It is to belong to typical three-dimensional netted nano-porous structure.Pore distribution is uniformly and intensive simultaneously, and also provable its has higher Porosity；
It carries out Fourier infrared (FTIR) to hydrophobic silica aerogel made from the present embodiment to be analyzed and characterized, as a result such as Fig. 3 It is shown；From figure 3, it can be seen that in 2961 cm of wave number-1Place is Si-CH3Stretching vibration peak；In 1096 cm-1Locate strong and wide Peak is Si-O-Si vibration peak.As can be seen that the tridimensional network that the aeroge is made of a large amount of Si-O-Si, while also having With the presence of many methyl for playing hydrophobic effect.
Embodiment 2:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) after 1:2 is mixed by volume, being added dropwise to concentration by 2 drops/s speed is 2.5mol/L for industrial-grade sodium silicate solution and water Aqueous hydrochloric acid solution be adjusted to pH value be 4, then pour into beaker together, be stirred to form silica solution, in silica solution press volume Dehydrated alcohol is added than 1:1.5 to continue to stir 5min, obtains mixture；
2) in the mixture of step 1), be slowly added dropwise into concentration be 0.6mol/L dilute ammonia solution be adjusted to pH value be 8.5(be added dropwise speed Degree is 2 drops/s), it stands after sol liquid in beaker gradually solidifies, the beaker is placed in 50 DEG C of water-bath, heated 40min carries out aging, forms blocky gel in beaker；
3) the blocky gel obtained after step 2 aging is pulverized, the deionized water (quality and deionized water of blocky gel is added Volume ratio 1:2), 2h is followed by stirring and washing, filter, filter residue immerse dehydrated alcohol in stirring 1h carry out exchange of solvent after (filter residue Quality and the ratio of volume of the dehydrated alcohol be 1:1.5), then filtered, filter residue, which immerses, stirs 1h(filter residue in modification liquid Immerse in modification liquid, the ratio of the volume of the quality of the filter residue and the modification liquid is 1:2), obtain modified mixed liquor；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, by volume 1: 1.5 are immersed in n-hexane after agitator treating 40min, are filtered, filter residue constant pressure and dry 1h at 70 DEG C, obtain described dredge Water aerosil.
Embodiment 3:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) hydrochloric acid water for being 2mol/L into concentration is slowly added dropwise after 1:1.5 is mixed by volume in industrial-grade sodium silicate solution and water It is 3(rate of addition is 2 drops/s that solution, which is adjusted to pH value), it then pours into beaker together, is stirred to form silica solution, silica solution In by volume 1:1.2 be added dehydrated alcohol continue stir 10min, obtain mixture；
2) in the mixture of step 1), being slowly added dropwise into concentration is that be adjusted to pH value be 8(rate of addition to 0.6mol/L dilute ammonia solution It for 2 drops/s), stands after sol liquid in beaker gradually solidifies, the beaker is placed in 45 DEG C of water-bath, heat 30min, Aging is carried out, forms blocky gel in beaker；
3) the blocky gel obtained after step 2 aging is pulverized, the deionized water (quality and deionized water of blocky gel is added Volume ratio 1:1.5), 1.5h is followed by stirring and washing, filter, filter residue immerse dehydrated alcohol in stirring 1h carry out exchange of solvent after (ratio of the quality of filter residue and the volume of the dehydrated alcohol is 1:1), then filtered, filter residue, which immerses in modification liquid, stirs 0.5h (filter residue immerses in modification liquid, and the ratio of the volume of the quality of the filter residue and the modification liquid is 1:1.7), obtains modified mixed liquor；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, 1:1 by volume It is immersed in n-hexane after agitator treating 30min, is filtered, filter residue constant pressure and dry 1h at 65 DEG C is obtained described hydrophobic Aerosil.
Embodiment 4:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) industrial-grade sodium silicate solution and water are slowly added dropwise water-soluble into the hydrochloric acid that concentration is 2mol/L after 1:2 is mixed by volume It is 2(rate of addition is 2 drops/s that liquid, which is adjusted to pH value), it then pours into beaker together, is stirred to form silica solution, in silica solution 1:1.3 is added dehydrated alcohol and continues to stir 12min by volume, obtains mixture；
2) in the mixture of step 1), being slowly added dropwise into concentration is that be adjusted to pH value be 8(rate of addition to 0.5mol/L dilute ammonia solution It for 2 drops/s), stands after sol liquid in beaker gradually solidifies, the beaker is placed in 45 DEG C of water-bath, heat 35min, Aging is carried out, forms blocky gel in beaker；
3) the blocky gel obtained after step 2 aging is pulverized, the deionized water (quality and deionized water of blocky gel is added Volume ratio 1:1.8), 1.5h is followed by stirring and washing, filter, filter residue immerse dehydrated alcohol in stirring 1h carry out exchange of solvent after (ratio of the quality of filter residue and the volume of the dehydrated alcohol is 1:1.2), then filtered, filter residue, which immerses in modification liquid, to be stirred 0.5h(filter residue immerses in modification liquid, and the ratio of the volume of the quality of the filter residue and the modification liquid is 1:1.3), obtain modified mixing Liquid；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, by volume 1: 1.1 are immersed in n-hexane after agitator treating 20min, are filtered, filter residue constant pressure and dry 1h at 70 DEG C, obtain described dredge Water aerosil.
Comparative example 1:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) hydrochloric acid water for being 2mol/L into concentration is slowly added dropwise after 1:1.5 is mixed by volume in industrial-grade sodium silicate solution and water It is 3(rate of addition is 2 drops/s that solution, which is adjusted to pH value), it then pours into beaker together, is stirred to form silica solution, silica solution In by volume 1:1.2 be added dehydrated alcohol continue stir 10min, obtain mixture；
2) in the mixture of step 1), being slowly added dropwise into concentration is that be adjusted to pH value be 8(rate of addition to 0.6mol/L dilute ammonia solution It for 2 drops/s), stands after sol liquid in beaker gradually solidifies, the beaker is placed in 45 DEG C of water-bath, heat 30min, Aging is carried out, forms blocky gel in beaker；
3) it after pulverizing the blocky gel obtained after step 2 aging, immerses in dehydrated alcohol and stirs 1 hour progress exchange of solvent (ratio of the volume of the quality and dehydrated alcohol of blocky gel is 1:1.5), filters, and filter residue immerses stirring 0.5h(filter in modification liquid Slag immerses in modification liquid, and the ratio of the volume of the quality of the filter residue and the modification liquid is 1:1.7), obtain modified mixed liquor；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, 1:1 by volume It is immersed in n-hexane after agitator treating 30min, is filtered, filter residue constant pressure and dry 1h at 65 DEG C is obtained described hydrophobic Aerosil.
Comparative example 2:
Prepare hydrophobic silica aerogel, comprising the following steps:
1) industrial-grade sodium silicate solution and water are slowly added dropwise water-soluble into the hydrochloric acid that concentration is 2mol/L after 1:2 is mixed by volume It is 2(rate of addition is 2 drops/s that liquid, which is adjusted to pH value), it then pours into beaker and stirs together, obtain silica solution；
2) in the silica solution of step 1), being slowly added dropwise into concentration is that be adjusted to pH value be 8(rate of addition to 0.5mol/L dilute ammonia solution It for 2 drops/s), stands after sol liquid in beaker gradually solidifies, the beaker is placed in 45 DEG C of water-bath, heat 35min, Aging is carried out, forms blocky gel in beaker；
3) the blocky gel obtained after step 2 aging is pulverized, the deionized water (quality and deionized water of blocky gel is added Volume ratio 1:1.8), agitator treating 1.5 hours, the gel particle after washing is filtered, filter residue immerse dehydrated alcohol in 1h is stirred filter, filter residue immerses after exchange of solvent (ratio of the quality of filter residue and the volume of the dehydrated alcohol is 1:1.2) It stirs 0.5h(filter residue in modification liquid to immerse in modification liquid, the ratio of the volume of the quality of the filter residue and the modification liquid is 1: 1.1) modified mixed liquor, is obtained；
4) by the modification mixed liquor stratification of step 3), upper liquid after taking the modified mixed liquor layering, by volume 1: 1.1 are immersed in n-hexane after agitator treating 20min, are filtered, filter residue constant pressure and dry 1h at 70 DEG C, obtain described dredge Water aerosil.
The hydrophobic silica aerogel prepared to embodiment 1 ~ 4 and comparative example 1 ~ 2 is tested for the property, and detects its jolt ramming Density, average pore size and porosity, testing result are as shown in table 1；The examination criteria of tap density is GB/T 21354- in table 1 2008。
The performance parameter of 1 hydrophobic silica aerogel of table
Grouping Tap density Average pore size Porosity
Embodiment 1 0.149g/cm3 20nm 94%
Embodiment 2 0.164g/cm3 20nm 93%
Embodiment 3 0.152g/cm3 30nm 93%
Embodiment 4 0.160g/cm3 30nm 93%
Comparative example 1 0.347g/cm3 Less porous 84%
Comparative example 2 0.423g/cm3 Less porous 81%
Aerogel products obtained by comparative example 1 ~ 2, sample have the phenomenon that obvious jaundice.
As can be drawn from Table 1, aerogel products density obtained by comparative example 1 ~ 2 is larger, and porosity is lower, this is because Without using deionized water in comparative example 1, inorganic salts remaining in gel duct are washed, cause to change in surface hydrophobicity Property step in hydrophobic grouping cannot be connected to channel surfaces well so that product is in the drying process because the presence of water causes Gel duct collapses；A certain amount of dehydrated alcohol is not added in the step 1) of comparative example 2 into colloidal sol, leads to gel bone obtained Frame is thiner, and product cannot bear solvent in the drying process and evaporate brought surface tension, and gel duct is caused to collapse. This explanation a certain amount of dehydrated alcohol is added when preparing hydrophobic silica aerogel and in gel duct into colloidal sol The washing operation of inorganic salts is very necessary；
And the embodiment of the present invention 1 ~ 4 the results show that the method limited through the invention, can be with cheap industrial waterglass Raw material, and the time of preparation is greatly reduced, improve production efficiency, hydrophobic silica aerogel tap density obtained 0.164g/cm3Hereinafter, average pore size is not more than 30nm, 93% or more porosity.
Content described in this specification is only to enumerate to inventive concept way of realization, and protection scope of the present invention is not answered When the concrete form for being seen as limited by embodiment and being stated, protection scope of the present invention is also only in those skilled in the art's root According to present inventive concept it is conceivable that equivalent technologies mean.

Claims (10)

1. a kind of method for preparing hydrophobic silica aerogel as the supper-fast normal pressure of raw material using waterglass, it is characterised in that including Following steps:
1) water glass solution is mixed with water, being slowly added dropwise into aqueous hydrochloric acid solution to pH value is 2 ~ 4, then pours into beaker together In, it is stirred to form silica solution, dehydrated alcohol is added, continues to stir, obtains mixture；
2) being slowly added dropwise in the mixture of step 1) and being adjusted to pH value into dilute ammonia solution is 7 ~ 8.5, is stood to sol liquid gradually After solidification, the beaker is placed in 40 ~ 50 DEG C of water-bath, heats 20 ~ 40min, carry out aging, formed in beaker blocky solidifying Glue；
3) the blocky gel obtained after step 2 aging is pulverized, 1 ~ 2h of deionized water agitator treating is added, is filtered, filter residue It immersing 0.5 ~ 1.5h of stirring in dehydrated alcohol and carries out exchange of solvent, then filtered, filter residue, which immerses, stirs 0.5 ~ 1h in modification liquid, Mixed liquor must be modified；
4) by the modification mixed liquor stratification of step 3), upper liquid is taken to be immersed in n-hexane after 20 ~ 40min of agitator treating, It is filtered, filter residue constant pressure and dry obtains the hydrophobic silica aerogel.
2. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 1), the volume ratio that water glass solution is mixed with water is 1:1 ~ 2.
3. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 1), the volume ratio of silica solution and dehydrated alcohol is 1:1 ~ 5, is added in the silica solution anhydrous Ethyl alcohol stirs 5 ~ 15min.
4. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 1), the concentration of aqueous hydrochloric acid solution is 1.5 ~ 2.5mol/L, preferably 2mol/L；The hydrochloric acid The rate of addition of aqueous solution is 2 drops/s.
5. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 2, the concentration of dilute ammonia solution is 0.2 ~ 0.6mol/L；The dropwise addition speed of the dilute ammonia solution Degree is 2 drops/s.
6. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 3), the quality of the blocky gel after pulverizing and the volume ratio of deionized water are 1:1 ~ 2, wherein The unit of quality is g, volume unit mL.
7. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that when being stirred in filter residue immersion dehydrated alcohol in step 3), the volume of the quality and dehydrated alcohol of filter residue Than for 1:0.7 ~ 1.5, wherein the unit of quality is g, volume unit mL.
8. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 3), modification liquid is the mixed liquor being made of n-hexane and trim,ethylchlorosilane；The modification liquid In, the volume ratio of n-hexane and trim,ethylchlorosilane is 8 ~ 12:1, preferably 10:1；Filter residue, which immerses in the modification liquid, to be stirred When, the ratio of the volume of the quality and modification liquid of filter residue is 1:1 ~ 2, and wherein the unit of quality is g, volume unit mL.
9. according to claim 1 a kind of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that in step 4), the volume ratio of upper liquid and n-hexane is 1:0.5 ~ 1.5.
10. one kind according to claim 1 prepares hydrophobic silica aerogel by the supper-fast normal pressure of raw material of waterglass Method, it is characterised in that the tap density of hydrophobic silica aerogel made from step 4) be 0.149 ~ 0.164g/cm3, Porosity is 93 ~ 94%, and average pore size is 20-30 nm.
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