CN108358212A - The preparation method and silica aerogel particles of silica aerogel particles - Google Patents
The preparation method and silica aerogel particles of silica aerogel particles Download PDFInfo
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- CN108358212A CN108358212A CN201810512120.8A CN201810512120A CN108358212A CN 108358212 A CN108358212 A CN 108358212A CN 201810512120 A CN201810512120 A CN 201810512120A CN 108358212 A CN108358212 A CN 108358212A
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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
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- 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
- C01P2006/10—Solid density
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- 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
- C01P2006/12—Surface area
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- 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
- C01P2006/14—Pore volume
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- 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
Abstract
The present invention relates to a kind of preparation methods of silica aerogel particles.The method is：Using cheap inorganic silicon source as raw material, Silica hydrogel is prepared by sol-gel technology, ripening is carried out to Silica hydrogel, acidification is carried out to Silica hydrogel with hydrochloric acid solution or hydrogen chloride gas, Rapid Alkylation Under modification is carried out to Silica hydrogel with organic siloxanes again, rapid draing is then carried out to alkylated Silica hydrogel using unique microwave tiny structure mode.This method, which prepares silica aerogel particles, has the characteristics that the modification time is short, drying time is short, use cheap Ludox for raw material simultaneously, it is particularly suitable for silica aerogel particles large-scale industrial production, is conducive to improve production efficiency, reduces overall cost.
Description
Technical field
The present invention relates to the preparation methods and silica of chemical field more particularly to a kind of silica aerogel particles
Aerogel particle.
Background technology
Silica aerogel particles are a kind of light nanoporous amorphous solid materials that heat preservation and insulation is very excellent
Material, porosity are up to 80%~99.8%, and the typical sizes of hole are 1~100nm, and specific surface area reaches as high as 1000m2/g
More than, room temperature thermal coefficient can be the minimum solid material of current thermal coefficient, can be described as super down to 0.013W/ (mk)
Heat-insulating material.Since silica aerogel particles heat preservation and insulation is apparently higher than Conventional insulation, make it in space flight, army
Work, metallurgy, petrochemical industry, energy saving building, solar energy composite such as utilize to be widely used at the fields.
Silica aerogel particles typical production process is divided into supercritical drying and atmosphere pressure desiccation.Supercritical drying
Method generally using organosilicon as silicon source, including methyl orthosilicate (TMOS), ethyl orthosilicate (TEOS), multi-polysiloxane (E-40) and
Other organosiloxanes etc. make solvent with absolute ethyl alcohol, and alcogel is prepared by sol-gel technology, then use overcritical
Seasoning prepares silica aerogel particles.Atmosphere pressure desiccation is generally using inorganic silicon as silicon source, including industrial waterglass, acidity
Ludox, alkaline silica sol etc. prepare hydrogel with water as solvent by sol-gel technology, then use low surface tension molten
Agent carries out solvent replacement to gel, is then alkylated and is changed to the hydrogel with trim,ethylchlorosilane or hexamethyldisilazane
Property processing, finally through constant pressure and dry legal system prepared silicon dioxide aerogel particle.Application publication number CN201610963506.1 patents
A kind of hydrophobic type silica aerogel particles and preparation method thereof are disclosed, with ethyl orthosilicate, methyltriethoxysilane
For co-precursor, ethyl alcohol is solvent, and water is hydrolytic reagent, and sodium hydroxide solution is catalyst, adds the second of fc-surfactant
Alcohol is Ageing solution, and the bulk silicon dioxide aerogel particle with good hydrophobic rate is made through supercritical drying process.Application is public
Cloth CN201510343705.8 patents disclose a kind of corrosion-free SiO2The preparation method of aerogel particle, using collosol and gel
Industrial waterglass is exchanged removal Na by two-step method with the mixed liquor of deionized water through weak-acid cation-exchange resin+, obtain pH
=3.0~4.0 colloidal sol, colloidal sol is adjusted pH value with ammonium hydroxide to obtain wet gel after standing, then wet gel is placed in positive silicon
Wet gel after aging is placed in progress solvent displacement in ethyl alcohol, then by solvent by aging in the Ageing solution of acetoacetic ester and ethyl alcohol
Exchanged wet gel is placed in the mixed liquor of hexamethyldisilazane and ethyl alcohol and is surface modified, and wet gel is after modified
It is placed in again in ethyl alcohol and carries out second of solvent displacement, finally wet gel is placed in CO 2 supercritical drying kettle and carries out super face
Silica aerogel particles are made in boundary's drying.Granted patent CN200910073009.4 discloses a kind of constant pressure and dry preparation
SiO2The method of aerogel particle, using ethyl orthosilicate as silicon source, through collosol and gel, aging, solvent displacement, surface modification, clear
Wash and constant pressure and dry processing after obtain SiO2Aerogel particle.Granted patent CN 201410025590.3 discloses one kind
The method that normal pressure prepares low-density bigger serface silica aerogel particles, this method is to be with cheap industrial waterglass
Presoma, absolute ethyl alcohol be solvent respectively in acid, be hydrolyzed under base catalysis, polycondensation reaction, obtain wet gel, it is dry to carry out water-bath
Dry aging, multiple exchange of solvent are classified after surface-modified and are dried to obtain low-density silicon dioxide aerogel particle under normal pressure.
Currently, preparing silica aerogel particles in process of production all using supercritical drying and atmosphere pressure desiccation
Face respective problem：Supercritical drying needs with high pressure resistant reaction kettle, to be typically designed 10~30MPa of pressure resistance, belongs to special equipment,
Fabrication cycle length, investment are big, and there is certain danger in operational process, and equipment investment is surprising if production capacity to be improved；Normal pressure
Seasoning solvent replaces time length (general 1~2 day, some meetings are longer), alkylation modification processing time length (20~48h), no
Drying time length (6~10h) is classified under synthermal gradient so that the entire silica aerogel particles production cycle is long, production
Inefficiency.
Invention content
Present invention aims at provide a kind of method that is inexpensive, quickly preparing silica aerogel particles, titanium dioxide
The manufacturing cycle of aerogel particles greatly shortens, while the manufacturing cost of silica aerogel particles is greatly reduced, favorably
In large-scale industrial production.
The method that a kind of low cost of the present invention quickly prepares silica aerogel particles, includes the following steps：
(1) it prepares：It prepares：By inorganic silicon source, alcohols solvent, deionized water with 1:(0~2):The volume of (0.2~0.7)
Percentage is uniformly mixed and forms mixed liquor, then carries out catalytic treatment to the mixed liquor with acid solution tune pH value, it is molten that silicon is made
Glue presoma；The inorganic silicon source is alkaline silica sol (JN-30) or industrial waterglass (modulus 3.0~3.3).The alcohols is molten
Agent is one or more mixed solutions in methanol, ethyl alcohol, propyl alcohol, ethylene glycol, glycerine.The acid solution is hydrochloric acid, sulphur
One or more mixed solutions in acid, nitric acid, hydrofluoric acid, acetic acid, oxalic acid.
(2) gel：The Ludox presoma is stood into 10~90min, forms Silica hydrogel.
(3) it is aged：By 1~8h of the Silica hydrogel room temperature, ripening is carried out.
(4) it is acidified：The Silica hydrogel after ageing is subjected to acidification.The step of acidification includes：Use salt
Acid solution impregnates the Silica hydrogel, and soaking time is 1~3h, and wherein concentration of hydrochloric acid solution is 20%~36%；Or use chlorination
Hydrogen to the Silica hydrogel carry out cycle purge, 5~60min of purge time, wherein chlorine hydride gas concentration be 90~
99.9vol%, the 5~30cm/s of gas flow rate.
(5) modified：：It is 1~5h, soaking temperature that the Silica hydrogel after acidification, which is put into soaking time in organic siloxanes,
50 DEG C~100 DEG C, carry out Rapid Alkylation Under modification.The organic siloxanes is methyltrimethoxysilane, methyl three
Ethoxysilane, trimethylmethoxysilane, trimethylethoxysilane, hexamethyldisiloxane, dimethylformamide dimethyl oxygroup silicon
One or more mixed solutions in alkane, dimethyl diethoxysilane.
(6) dry：Microwave tiny structure drying process is carried out to the modified Silica hydrogel, obtains aerosil
Particle.The microwave tiny structure drying power is 80~150KW, and vacuum degree is 400~600 supports during drying, and drying temperature is
60~120 DEG C, drying time is 15~60min.
Preferably, the alcohols solvent is ethyl alcohol, and the acid solution is hydrochloric acid.
Preferably, the gel time is 30min, and the digestion time is 2h.
Preferably, when the ageing selects hydrochloric acid solution to impregnate Silica hydrogel, soaking time 1h, concentration of hydrochloric acid solution is
25%.
Preferably, when the ageing selects hydrogen chloride gas to carry out cycle purge to Silica hydrogel, the purge time is
30min, chlorine hydride gas concentration 99.9vol%, gas flow rate 25cm/s.
Preferably, in the modifying process, organic siloxanes is hexamethyldisiloxane, soaking time 2.5h, leaching
It is 60 DEG C to steep temperature.
Preferably, in the drying process, dry power is 135KW, and vacuum degree is 450 supports, and drying temperature is 110 DEG C,
Drying time is 30min.
The present invention also provides a kind of silica aerogel particles, the silica aerogel particles are by above-mentioned preparation
Prepared by method, the apparent densities of the silica aerogel particles is 0.11~0.18g/cm3, and specific surface area is 500~
925m2/g, pore volume are 2.1~3.8cm3/g, and average pore size is 19~22nm.
The preparation method of silica aerogel particles provided by the invention, using microwave tiny structure drying mode, significantly
The manufacturing cycle of silica aerogel particles is shortened, while using inorganic silicon source for raw material, also makes aerosil
The manufacturing cost of particle substantially reduces, and is conducive to large-scale industrial production.
Meanwhile the preparation method of silica aerogel particles of the present invention, it solves non-pressure process technique and deposits at present
Solvent replace the problems such as time is long, alkylation modification processing time is long and drying time is long, substantially reduce silica
The manufacturing cycle of aerogel particle is conducive to the large-scale industrial production of silica aerogel particles.Side of the present invention
The apparent density of silica aerogel particles prepared by method is 0.11~0.18g/cm3, specific surface area is 500~925m2/ g,
Pore volume is 2.1~3.8cm3/ g, average pore size are 19~22nm, and index parameter is good, and product quality is high.
Description of the drawings
Fig. 1 show the process flow chart that low cost provided by the invention quickly prepares silica aerogel particles.
Specific implementation mode
The method of the present invention, which prepares silica aerogel particles, has the characteristics that the modification time is short, drying time is short,
Be conducive to improve production efficiency, reduce overall cost, is suitble to scale, industrialized production.It is illustrated below with specific example：
Embodiment 1
(1) it prepares：Under magnetic stirring by 10ml alkaline silica sols (JN-30), 15ml absolute ethyl alcohols and 5ml deionized waters
Uniformly mixing, the hydrochloric acid solution that 0.1mol/L is added adjust pH=8.5, Ludox presoma are made；
(2) gel：Above-mentioned presoma is stood into 30min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：The Silica hydrogel after ageing, soaking time 1h, after the completion discharge in time are impregnated with 25% hydrochloric acid solution
Hydrochloric acid realizes acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 50ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.18g/cm3, specific surface area is
515m2/ g, pore volume 2.1cm3/ g, average pore size 19nm.
Embodiment 2
(1) it prepares：Under magnetic stirring by 10ml alkaline silica sols (JN-30), 15ml absolute ethyl alcohols and 5ml deionized waters
Uniformly mixing, the acetic acid solution that 0.1mol/L is added adjust pH=8.5, Ludox presoma are made；
(2) gel：Above-mentioned presoma is stood into 40min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：The Silica hydrogel after ageing, soaking time 1h, after the completion discharge in time are impregnated with 25% hydrochloric acid solution
Hydrochloric acid realizes acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 50ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.17g/cm3, specific surface area is
553m2/ g, pore volume 2.5cm3/ g, average pore size 22nm.
Embodiment 3
(1) it prepares：Under magnetic stirring by 10ml alkaline silica sols (JN-30), 15ml absolute ethyl alcohols and 5ml deionized waters
Uniformly mixing, the hydrochloric acid solution that 0.1mol/L is added adjust pH=8.5, Ludox presoma are made；
(2) gel：Above-mentioned presoma is stood into 30min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：Cycle purge is carried out to Silica hydrogel after ageing with hydrogen chloride gas, chlorine hydride gas concentration is
99.9vol%, gas flow rate 25cm/s, purge time 30min realize acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 50ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.16g/cm3, specific surface area is
524m2/ g, pore volume 2.4cm3/ g, average pore size 21nm.
Embodiment 4
(1) it prepares：Under magnetic stirring by 10ml alkaline silica sols (JN-30), 15ml absolute ethyl alcohols and 5ml deionized waters
Uniformly mixing, the acetic acid solution that 0.1mol/L is added adjust pH=8.5, Ludox presoma are made；
(2) gel：Above-mentioned presoma is stood into 40min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：Cycle purge is carried out to Silica hydrogel after ageing with hydrogen chloride gas, chlorine hydride gas concentration is
99.9vol%, gas flow rate 25cm/s, purge time 30min realize acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 50ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.14g/cm3, specific surface area is
582m2/ g, pore volume 2.9cm3/ g, average pore size 20nm.
Embodiment 5
(1) it prepares：10ml industrial waterglass (modulus 3.1) is uniformly mixed under magnetic stirring with 40ml deionized waters,
The acetic acid solution that 0.1mol/L is added adjusts pH=11, and Ludox presoma is made；
(2) gel：Above-mentioned presoma is stood into 30min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：The Silica hydrogel after ageing, soaking time 1h, after the completion discharge in time are impregnated with 25% hydrochloric acid solution
Hydrochloric acid realizes acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 70ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.12g/cm3, specific surface area is
912m2/ g, pore volume 3.6cm3/ g, average pore size 22nm.
Embodiment 6
(1) it prepares：10ml industrial waterglass (modulus 3.1) is uniformly mixed under magnetic stirring with 40ml deionized waters,
The acetic acid solution that 0.1mol/L is added adjusts pH=11, and Ludox presoma is made；
(2) gel：Above-mentioned presoma is stood into 30min, forms Silica hydrogel；
(3) it is aged：Silica hydrogel is placed into 2h at normal temperatures, carries out ripening；
(4) it is acidified：Cycle purge is carried out to Silica hydrogel after ageing with hydrogen chloride gas, chlorine hydride gas concentration is
99.9vol%, gas flow rate 25cm/s, purge time 30min realize acidification；
(5) modified：The Silica hydrogel after acidification, 60 DEG C of soaking temperature, soaking time are impregnated with 70ml hexamethyldisiloxane
2.5h carries out Rapid Alkylation Under modification；
(6) dry：To modified Silica hydrogel carry out tiny structure drying, 110 DEG C of drying temperature, microwave drying power 135KW,
450 support of vacuum degree during drying, drying time 30min obtain silica aerogel particles.
The apparent density of the silica aerogel particles prepared through the above steps is 0.11g/cm3, specific surface area is
925m2/ g, pore volume 3.8cm3/ g, average pore size 20nm.
The above is the specific implementation mode of the present invention, it is noted that for those skilled in the art
For, without departing from the principle of the present invention, several improve and perfects can also be made, these improve and perfects are also considered as
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silica aerogel particles, it is characterised in that：Described method includes following steps：
(1) it prepares：By inorganic silicon source, alcohols solvent, deionized water with 1:(0~2):The percent by volume of (0.2~0.7) mixes
It is formed uniformly mixed liquor, catalytic treatment then is carried out to the mixed liquor with acid solution tune pH value, Ludox presoma is made；
(2) gel：The Ludox presoma is stood, Silica hydrogel is formed；
(3) it is aged：The Silica hydrogel is placed into a period of time, carries out ripening；
(4) it is acidified：The Silica hydrogel after ageing is subjected to acidification；
(5) modified：The Silica hydrogel after acidification is put into organic siloxanes and is impregnated, is carried out at Rapid Alkylation Under modification
Reason；
(6) dry：Microwave tiny structure drying process is carried out to the modified Silica hydrogel, obtains aerosil
Grain.
2. according to the method described in claim 1, it is characterized in that：The inorganic silicon source is that industrial waterglass or alkaline silicon are molten
Glue.
3. according to the method described in claim 1, it is characterized in that：The alcohols solvent be methanol, ethyl alcohol, propyl alcohol, ethylene glycol,
One or more mixed solutions in glycerine.
4. according to the method described in claim 1, it is characterized in that：The acid solution is hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, second
One or more mixed solutions in acid, oxalic acid.
5. according to the method described in claim 1, it is characterized in that：The Ludox presoma pH value is 6~11.
6. according to the method described in claim 1, it is characterized in that：The step of acidification includes：It is soaked with hydrochloric acid solution
The Silica hydrogel is steeped, soaking time is 1~3h, and wherein concentration of hydrochloric acid solution is 20%~36%；Or with hydrogen chloride gas pair
The Silica hydrogel carries out cycle purge, and 5~60min of purge time, wherein chlorine hydride gas concentration are 90~99.9vol%, institute
State 5~30cm/s of gas flow rate.
7. according to the method described in claim 1, it is characterized in that：The organic siloxanes be methyltrimethoxysilane,
Methyltriethoxysilane, trimethylmethoxysilane, trimethylethoxysilane, hexamethyldisiloxane, dimethylformamide dimethyl
One or more mixed solutions in oxysilane, dimethyl diethoxysilane.
8. according to the method described in claim 1, it is characterized in that：The Silica hydrogel after acidification is put into organic siloxanes
Soaking time is 1~5h, 50 DEG C~100 DEG C of soaking temperature.
9. according to the method described in claim 1, it is characterized in that：The microwave tiny structure drying power is 80~150KW, is done
Dry period vacuum degree is 400~600 supports, and drying temperature is 60~120 DEG C, and drying time is 15~60min.
10. a kind of silica aerogel particles, which is characterized in that the silica aerogel particles are by claim 1~9
It is prepared by the preparation methods of the silica aerogel particles described in any one, the silica aerogel particles it is apparent close
Degree is 0.11~0.18g/cm3, specific surface area is 500~925m2/ g, pore volume are 2.1~3.8cm3/ g, average pore size 19
~22nm.
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Application publication date: 20180803 |