CN107857273A - The device of automatic replacing solvent in a kind of hydrophobic silicon dioxide aerogel preparation process - Google Patents
The device of automatic replacing solvent in a kind of hydrophobic silicon dioxide aerogel preparation process Download PDFInfo
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- CN107857273A CN107857273A CN201711249860.9A CN201711249860A CN107857273A CN 107857273 A CN107857273 A CN 107857273A CN 201711249860 A CN201711249860 A CN 201711249860A CN 107857273 A CN107857273 A CN 107857273A
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- solvent
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- wet gel
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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
- 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
- C01B33/152—Preparation of hydrogels
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of device of automatic replacing solvent in hydrophobic silicon dioxide aerogel preparation process, described device includes cylindrical reactor, condenser (1) is installed on cylindrical reactor, cylindrical reactor is divided into upper and lower two layers, upper strata is used to react into line replacement, lower floor is used to place recycling design, and circulation loop is formed by return duct (6), steam pipe (3) between upper and lower layer and condenser (1).The present invention is directed to the device that automatic replacing solvent in a kind of preparation process is provided in place of the deficiencies of solvent displacement is repeatedly, the consuming time is long during preparing hydrophobic silicon dioxide aerogel, automatic replacing solvent can be realized using the device, and solvent can recycle, self-emptying can also be realized, it is time saving and energy saving.
Description
Technical field
The present invention relates to a kind of device of automatic replacing solvent in hydrophobic silicon dioxide aerogel preparation process, Yi Jili
The method that hydrophobic silicon dioxide aerogel is prepared with the device.
Background technology
Aeroge is a kind of advanced extremely-low density material, according to nanostructured and the species of initiation material, its porosity
For 90% or higher, specific surface area is hundreds of m2/ g to 1500m2/g.Nanoporous aerogel can be used for such as ultralow dielectric
Material, catalyst, electrode material and acoustic material application in, especially, the low aerosil of heat transfer degree
It is that can be used in refrigerator, automobile, aircraft and other application.
The solvent being full of in its network hole of the silica wet gel obtained through Ludox polycondensation is mainly water, due to water
Surface tension it is very big (72dyn/cm), therefore the additonal pressure of capillary in the drying process is very big, it is not easy to is evaporated, often
Press dry it is dry during phenomenon due to bearing incessantly surface tension of liquid and occurring shrinking or cave in just occurs, this is to cause gas
Ftracture broken immediate cause in gel preparation course.If replaced by solvent, water is replaced with surface tension small solvent
Out, during the small solvent evaporation drying of these surface tension, additonal pressure will greatly reduce, to realizing prepared by extremal stability
Aeroge is highly advantageous.Surface tension H2O(72dyn/cm)>Acetone (26.26)>Ethanol (24.05dyn/cm)>Hexane
(20.44dyn/cm).Prepare at present during aerosil using traditional solvent method of replacing, it is necessary to repeatedly anti-
It is multiple, expend time length.
Patent CN103787343A discloses a kind of preparation method of the microspheric aeroge based on super hydrophobic surface, prepares production
Product and its application.The preparation method of the microspheric aeroge is small easily to be formed on super hydrophobic surface using silica aqueous solution
Ball, and further gel form wet gel, after by series of processes obtain finished product, process is overelaborated, while consumes and largely put
Change solvent.
Patent CN201380024768.6 discloses solvent-displacement solvent used in a kind of hydrophobization aeroge manufacture, and
It is directed to use with the solvent-displacement solvent hydrophobization aeroge manufacture method.Not only the moisture in wet gel is by solvent-displacement
Solvent is effectively replaced, and can easily and high-purity ground recycling design.The shortcomings that this method, can not determine displacement terminal,
Solvent loss rate can not reach minimum.
For during preparing hydrophobic silicon dioxide aerogel solvent displacement repeatedly, expend the time it is long the problems such as, this
Invention provides a kind of device of automatic replacing solvent in preparation process, and automatic replacing solvent can be realized using the device, and molten
Agent can recycle, additionally it is possible to self-emptying is realized, it is time saving and energy saving.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of hydrophobicity
The device of automatic replacing solvent in aerosil preparation process, realize that the solvent displacement of wet gel changes with hydrophobic automatically
Property, and the method for preparing according to the device hydrophobic silicon dioxide aerogel.
In order to solve the above technical problems, technical scheme provided by the invention is：
A kind of device of automatic replacing solvent in hydrophobic silicon dioxide aerogel preparation process is provided, described device includes
Cylindrical reactor, condenser (1) is installed on cylindrical reactor, cylindrical reactor is divided into upper and lower two layers, and upper strata is used for
Enter line replacement reaction, lower floor is used to place recycling design, passes through return duct (6), steam pipe between upper and lower layer and condenser (1)
(3) circulation loop is formed；
The return duct (6) is the bend pipe with siphonage, installed in the bottom on reactor upper strata and the top of lower floor
To connect upper strata bottom and lower floor, when the solvent of displacement reaction is reached at the top of return duct, the liquid on reactor upper strata can be automatic
Flow to reactor lower floor；
Steam pipe (3) the connection condenser (1) and reactor lower floor, and steam pipe (3) lower end is placed under reactor
Layer top, to be inverted triangular funnel shape.
By such scheme, the cylindrical reactor upper strata is additionally provided with charging aperture (2) and discharging opening (5), charging aperture (2)
Reactor top of the upper layer is arranged on, the middle part of sliding channel on reactor upper strata is embedded with open type wedge shape material guide groove (12), and discharging opening is with drawing
Hopper (12) closing in end is connected, and material guide groove (12) is at least partly designed as engraved structure, shape less than discharging opening horizontal position
Into filter screen (13).
By such scheme, the cylindrical reactor upper strata is additionally provided with Height Adjustable propeller agitator, promotes
The paddle of formula agitator is oblique leaf oar, and the blade setting height(from bottom) of propeller agitator is concordant with discharging opening (5).
By such scheme, valve (4) is also equipped with the discharging opening.
Preferably, bottom end of the return duct (6) on reactor upper strata is additionally provided with filter.Filter can prevent gel
Ball passes through return duct.
The present invention also provides the method that hydrophobic silicon dioxide aerogel is prepared according to said apparatus, and its step is as follows：
1) silica wet gel ball is prepared：Deionized water is mixed with Ludox or waterglass, is stirring evenly and then adding into
Ammoniacal liquor, regulation pH value obtain wet gel for 4~10, are then added dropwise by pin hole or wet gel is placed in ultraphobic water meter by spray regime
On face, then silica wet gel ball is obtained using sessile drop method；
2) hydrophobic silica wet gel ball is prepared：It is anti-that silica wet gel ball obtained by step 1) is added into cylinder
Answer in device upper strata, open propeller agitator, add solvent-displacement solvent, the solvent on cylindrical reactor upper strata gradually passes through
Return duct (6) is transferred to cylindrical reactor lower floor, then bottom of device is heated in the range of 70 DEG C~80 DEG C, solvent
Steam enters condenser (1) through steam pipe (3), condenses into liquid and flows into cylindrical reactor upper strata, be thusly-formed circulation 1~
2h, hydrophobic modifier then is added to cylindrical reactor upper strata, continue to circulate until that silica wet gel ball all floats
Discharging, material enter material guide groove under the drive of agitating paddle, while in discharging opening to obtain hydrophobic silica wet for Open valve
Gel ball；
3) hydrophobic silicon dioxide aerogel ball is prepared：The hydrophobic silica wet gel ball that step 2) is obtained is dried
Obtain hydrophobic silicon dioxide aerogel ball.
Preferably, the step 2) solvent-displacement solvent is n-hexane and acetone in mass ratio 45~95%：55~
5% mixture.
Preferably, the step 2) solvent-displacement solvent is n-hexane and ethanol in mass ratio 45~95%：55~
5% mixture.
Preferably, the step 2) hydrophobic modifier is trim,ethylchlorosilane, HMDS, the ethoxy of phenyl three
One kind in base silane.
Preferably, the hydrophobic modifier described in step 2) and the mol ratio of n-hexane in solvent-displacement solvent are 1：6~
10。
By such scheme, the stoving process condition described in step 3) is：24h is dried at room temperature for, then in 50 DEG C of dryings
1h, finally it is warming up to 150 DEG C of dry 2h.
The beneficial effects of the present invention are：1st, the present invention is directed to the solvent during hydrophobic silicon dioxide aerogel is prepared
The deficiencies of displacement is repeatedly, the consuming time is long part provides a kind of device of automatic replacing solvent in preparation process, utilizes the device
Automatic replacing solvent can be realized, and solvent can recycle, additionally it is possible to self-emptying is realized, it is time saving and energy saving.2nd, utilize
Device of the present invention, which prepares hydrophobic silicon dioxide aerogel, can make solvent loss reach minimum, and preparation technology letter
It is single.
Brief description of the drawings
Fig. 1 is that the device of automatic replacing solvent in the hydrophobic silicon dioxide aerogel preparation process of the embodiment of the present invention 1 shows
It is intended to；
Fig. 2 is the discharging schematic diagram of automatic replacing solvent in the hydrophobic silicon dioxide aerogel preparation process of embodiment 1.
Wherein：1- condensers；2- charging apertures；3- steam pipes；4- valves；5- discharging openings；6- return ducts；On 7- reactors
Layer；8- dividing plates；9- reactors lower floor；10- heaters；11- propeller agitators；12- material guide grooves；13- filter screens.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into
One step is described in detail.
Embodiment 1
Such as the device signal that Fig. 1 is automatic replacing solvent in the present embodiment hydrophobic silicon dioxide aerogel preparation process
Figure.The device includes cylindrical reactor, and condenser 1 is provided with cylindrical reactor, and cylindrical reactor is divided into upper and lower two
Layer, upper strata be used for into line replacement react, lower floor be used for place recycling design, between upper and lower layer and condenser 1 by return duct 6,
Steam pipe 3 forms circulation loop；
Return duct 6 is the bend pipe with siphonage, installed in the bottom on reactor upper strata and the top of lower floor to connect
Upper strata bottom and lower floor, when the solvent of displacement reaction is reached at the top of return duct, the liquid on reactor upper strata can flow to instead automatically
Device lower floor is answered, bottom end of the return duct 6 on reactor upper strata is additionally provided with filter.Filter can prevent gel ball from passing through return duct；
Steam pipe 3 connects condenser 1 and reactor lower floor, and the lower end of steam pipe 3 is placed in above reactor lower floor, to fall
Put triangular funnel shape.
Cylindrical reactor upper strata is additionally provided with charging aperture 2 and discharging opening 5, and charging aperture 2 is arranged on reactor top of the upper layer,
The middle part of sliding channel on reactor upper strata is embedded with open type wedge shape material guide groove 12, and discharging opening is connected with the closing in end of material guide groove 12, and draws
Hopper 12 is designed as engraved structure less than discharging opening horizontal component, forms filter screen 13.Aperture of filter screen is less than material, it is ensured that makes solvent
It can filter, material can flow out from discharging opening.
Cylindrical reactor upper strata is additionally provided with Height Adjustable propeller agitator, and the paddle of propeller agitator is
Oblique leaf oar, and the blade setting height(from bottom) of propeller agitator is concordant with discharging opening 5, enables material under the promotion of oblique leaf oar
Smoothly discharging.
The method that hydrophobic silicon dioxide aerogel is prepared using said apparatus, is comprised the following steps that：
1) silica wet gel ball is prepared：Measure 10mL SiO2Content is 40% acidic silicasol, adds 70mL and goes
Ionized water dilutes, and is stirring evenly and then adding into ammoniacal liquor, and regulation pH value is 6, obtains wet gel, then passes through pin hole dropwise addition or injection side
Wet gel is placed on both ultrahydrophobic by formula, then obtains silica wet gel ball using sessile drop method；
2) hydrophobic silica wet gel ball is prepared：It is anti-that silica wet gel ball obtained by step 1) is added into cylinder
Answer in device upper strata, open propeller agitator, adjustment agitator rotation direction is counterclockwise, so that drive of the material in agitating paddle
It is lower to enter reactor upper strata bottom, the mixed solvent of solvent-displacement solvent hexane and ethanol is added, wherein n-hexane quality is
495g, ethanol quality are 405g, and the solvent on cylindrical reactor upper strata gradually passes through return duct 6 and is transferred under cylindrical reactor
Layer, then bottom of device is carried out to be heated to 80 DEG C, solvent vapo(u)r enters condenser 1 through steam pipe 3, condenses into liquid and flows into circle
Cylindricality reactor upper strata, circulation 2h is thusly-formed, hydrophobic modifier trim,ethylchlorosilane 104g is then added, continues to circulate until
Silica wet gel ball all floats, and adjustment agitator rotation direction is clockwise, so that material can be in the band of agitating paddle
Enter material guide groove, while Open valve under dynamic, obtain hydrophobic silica wet gel ball in discharging opening, discharging schematic diagram is as schemed
Shown in 2；
3) hydrophobic silicon dioxide aerogel ball is prepared：The hydrophobic silica wet gel ball that step 2) is obtained is in room
Temperature is lower to dry 24h, and 1h is then dried at 50 DEG C, 150 DEG C of dry 2h is finally warming up to and obtains hydrophobic silicon dioxide aerogel
Ball.
Claims (9)
- A kind of 1. device of automatic replacing solvent in hydrophobic silicon dioxide aerogel preparation process, it is characterised in that：The dress To put including cylindrical reactor, condenser (1) is installed on cylindrical reactor, cylindrical reactor is divided into upper and lower two layers, on Layer be used for into line replacement react, lower floor be used for place recycling design, between upper and lower layer and condenser (1) by return duct (6), Steam pipe (3) forms circulation loop；The return duct (6) is the bend pipe with siphonage, installed in the bottom on reactor upper strata and the top of lower floor with even Layer bottom and lower floor are connected, when the solvent of displacement reaction is reached at the top of return duct, the liquid on reactor upper strata can flow to automatically Reactor lower floor；Steam pipe (3) the connection condenser (1) and reactor lower floor, and steam pipe (3) lower end is placed in reactor lower floor Side, to be inverted triangular funnel shape.
- 2. device according to claim 1, it is characterised in that：The cylindrical reactor upper strata is additionally provided with charging aperture (2) and discharging opening (5), charging aperture (2) are arranged on reactor top of the upper layer, and the middle part of sliding channel on reactor upper strata is embedded with open type wedge Shape material guide groove (12), discharging opening are connected with material guide groove (12) closing in end, and material guide groove (12) is at least partly less than discharging saliva Flat position is designed as engraved structure, forms filter screen (13).
- 3. device according to claim 2, it is characterised in that：The cylindrical reactor upper strata is additionally provided with height adjustable The propeller agitator of section, the paddle of propeller agitator are oblique leaf oar, and the blade setting height(from bottom) of propeller agitator with Discharging opening (5) is concordant.
- 4. device according to claim 2, it is characterised in that：Valve (4) is also equipped with the discharging opening.
- 5. a kind of method for preparing hydrophobic silicon dioxide aerogel using any described devices of claim 1-4, its feature exist It is as follows in step：1) silica wet gel ball is prepared：Deionized water is mixed with Ludox or waterglass, is stirring evenly and then adding into ammoniacal liquor, Regulation pH value obtains wet gel for 4~10, is then added dropwise by pin hole or wet gel is placed on both ultrahydrophobic by spray regime, Then silica wet gel ball is obtained using sessile drop method；2) hydrophobic silica wet gel ball is prepared：Silica wet gel ball obtained by step 1) is added into cylindrical reactor In upper strata, propeller agitator is opened, adds solvent-displacement solvent, the solvent on cylindrical reactor upper strata gradually passes through backflow Pipe (6) is transferred to cylindrical reactor lower floor, then bottom of device is heated in the range of 70 DEG C~80 DEG C, solvent vapo(u)r Enter condenser (1) through steam pipe (3), condense into liquid and flow into cylindrical reactor upper strata, be thusly-formed 1~2h of circulation, so Backward cylindrical reactor upper strata adds hydrophobic modifier, continues to circulate until that silica wet gel ball all floats and discharges, Material enters material guide groove under the drive of agitating paddle, while Open valve obtains hydrophobic silica wet gel in discharging opening Ball；3) hydrophobic silicon dioxide aerogel ball is prepared：The hydrophobic silica wet gel ball that step 2) obtains is dried to obtain Hydrophobic silicon dioxide aerogel ball.
- 6. preparation method according to claim 5, it is characterised in that the step 2) solvent-displacement solvent be n-hexane and Acetone in mass ratio 45~95%：55~5% mixture.
- 7. preparation method according to claim 5, it is characterised in that the step 2) solvent-displacement solvent be n-hexane and Ethanol in mass ratio 45~95%：55~5% mixture.
- 8. preparation method according to claim 5, it is characterised in that the step 2) hydrophobic modifier is trimethylchloro-silicane One kind in alkane, HMDS, phenyl triethoxysilane.
- 9. preparation method according to claim 5, it is characterised in that the stoving process condition described in step 3) is：In room temperature Lower dry 24h, then in 50 DEG C of dry 1h, finally it is warming up to 150 DEG C of dry 2h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534353A (en) * | 2018-12-24 | 2019-03-29 | 内蒙古大学 | A kind of fast preparation method of kaolin-methanol intercalated compound |
| CN111498857A (en) * | 2020-03-04 | 2020-08-07 | 赵国升 | Process for the preparation of silica aerogels |
| TWI726638B (en) * | 2020-03-02 | 2021-05-01 | 趙國昇 | Preparation method of silica aerogel |
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| CN103101917A (en) * | 2011-11-09 | 2013-05-15 | Emp有限公司 | Super hydrophobic silica aerogel powders |
| CN206328320U (en) * | 2016-10-28 | 2017-07-14 | 湖北三宁化工股份有限公司 | A kind of high purity caprolactam refining plant |
| CN107108237A (en) * | 2015-11-27 | 2017-08-29 | 株式会社Lg化学 | The preparation method of hydrophobic silicon dioxide aerogel and the hydrophobic silicon dioxide aerogel thus prepared |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
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| CN101274762A (en) * | 2007-03-29 | 2008-10-01 | 北京市华从经贸有限责任公司 | Modification method for silicon dioxide aerogel |
| CN103101917A (en) * | 2011-11-09 | 2013-05-15 | Emp有限公司 | Super hydrophobic silica aerogel powders |
| CN107108237A (en) * | 2015-11-27 | 2017-08-29 | 株式会社Lg化学 | The preparation method of hydrophobic silicon dioxide aerogel and the hydrophobic silicon dioxide aerogel thus prepared |
| CN206328320U (en) * | 2016-10-28 | 2017-07-14 | 湖北三宁化工股份有限公司 | A kind of high purity caprolactam refining plant |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI726638B (en) * | 2020-03-02 | 2021-05-01 | 趙國昇 | Preparation method of silica aerogel |
| CN111498857A (en) * | 2020-03-04 | 2020-08-07 | 赵国升 | Process for the preparation of silica aerogels |
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