CN106984062B - A kind of efficient complex compound wet gel solvent method of replacing - Google Patents
A kind of efficient complex compound wet gel solvent method of replacing Download PDFInfo
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- CN106984062B CN106984062B CN201710192411.9A CN201710192411A CN106984062B CN 106984062 B CN106984062 B CN 106984062B CN 201710192411 A CN201710192411 A CN 201710192411A CN 106984062 B CN106984062 B CN 106984062B
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- organic solvent
- gel
- wet gel
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- water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D12/00—Displacing liquid, e.g. from wet solids or from dispersions of liquids or from solids in liquids, by means of another liquid
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Colloid Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The invention discloses a kind of efficient complex compound wet gel solvent method of replacing, it is combined using heating stirring and cooling displacement, after observation wet gel is formed, the moisture in wet gel is sufficiently displaced from by heating, stirring and strict temperature control with the surface tension organic solvent lower than water；This method significantly shortens the time swap of complex compound gel solvent, promotes solvent displacement effect, and reduces the consumption of displacement solvent and the consumption of other energy resources, provides the complex compound solvent method of replacing that one kind is high-efficient, effect is good and economizes on resources.
Description
Technical field
The present invention relates to complex compound wet gel preparation technical field, specifically a kind of efficient complex compound wet gel solvent is set
Change method.
Background technique
Replacing solvent drying technique is that (including treated for washing filtering for aqueous solvent in the product that liquid phase method is prepared
Water/organic solvent) organic solvent (including liquid CO 2 or supercritical CO 2) replacement Treatment is carried out before it is dried, then using appropriate
Drying means and obtain a kind of operating method of nano material product.
Using wet chemistry method prepare nano-powder when, need in the preprocessing process such as filtering before it is dried, with water into
Row repeatedly washing, various foreign ions remaining in liquid phase are removed as far as possible, but in the drying process after washing, can not keep away
Exempt from that the reunion between powder granule can be caused.Because the solvent for gel is replaced, often required by subsequent drying process, institute
To remain in intergranular water with the surface tension organic solvent substitution lower than water, the preferable nano powder of dispersibility can be obtained
Body.Replace the process for remaining in intergranular water, as organic solvent displacement method with the surface tension organic solvent lower than water.
The organic solvent method of replacing used in science preparation process at present is infusion method and two kinds of washing method, specifically such as
Under:
1) infusion method: being cut into column for hydrogel, is put into the lesser organic solvent of surface tension and impregnates several hours, instead
Organic solvent is replaced again, after the moisture in gel is replaced by organic solvent, ultimately forms block-like organic solvent gel.
This immersion organic solvent displacement method takes a long time, larger to the consumption of organic solvent, and due to blocky water-setting
Colloid product is larger, surface area is smaller, and organic solvent is unable to fully cement out moisture, it is difficult to reach wanting for subsequent drying process
It asks.
2) washing method: after hydrogel being washed with deionized water repeatedly repeatedly, then with alcohol multipass is washed repeatedly.Subsequent drying
It dries to obtain than more loose block through baking oven in the process.
This washing organic solvent displacement method time-consuming is shorter but very big to the consuming of organic solvent, and is more difficult to
Except the moisture in hydrogel, it is unable to reach the requirement of subsequent drying process, causes the agglomeration between microscopic particles serious.
That there are commonly solvent method of replacing now is more coarse and simple and crude for both the above, leads to subsequent dry work
As a result barely satisfactory, it is difficult to which that the precision for meeting current material preparation accurately requires.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to and provide a kind of efficient complex compound wet gel solvent and set
Method is changed, this method time swap is short, and it is small to the consumption of organic solvent, it economizes on resources, displacement efficiency is high, effect is good.
Realizing the technical solution of the object of the invention is:
A kind of efficient complex compound wet gel solvent method of replacing is combined, specifically using heating stirring and cooling displacement
Include the following steps:
1) it observes the formation of wet gel: wet gel to be replaced is placed in container, container is placed under water bath with thermostatic control environment,
Magnetic agitation wet gel, when wet gel liquid level no longer at any time and heating stirring decline, that is, form preliminary wet gel；
2) organic solvent is added in preliminary wet gel into step 1), continues magnetic agitation 30 minutes, is formed new wet solidifying
Glue；
3) water bath is moved the containers out, the organic solvent of wet gel upper layer remnants new in step 2 is removed, again
Organic solvent is added；At room temperature, vertical direction is kept to stir gel colloidal along chamber wall with stirring rod, it will be on chamber wall
Stirrable gel stir into organic solvent, form a large amount of powders in container at this time, organic solvent displacement quickly occurs；
It is difficult to stir if 4) have residual gel on stirring rod or chamber wall and be hardened, container is put back in water-bath slightly
Heat takes out container, continues to stir under room temperature, 1-2 times repeatedly after gel softening can stir；
5) after gel is fully converted to the powder of fine uniform, container is taken out, organic solvent is drained, it then will be in container
Powder take out save；
By above-mentioned steps, complex compound wet gel is successfully replaced, entire replacement process total time-consuming is not more than 1 hour.
The temperature of the water bath with thermostatic control is 10 ~ 80 DEG C.
The organic solvent, surface tension are not more than 25 mN/m.
The organic solvent be dehydrated alcohol, acetone, methanol, normal propyl alcohol, n-butanol, methyl butanone, hexamethylene and
At least one of normal heptane.
In the step 4), when the water bath temperature of organic solvent setting is lower than room temperature, remained when being stirred at room temperature solidifying
Glue has originally softened, then it is not necessary that container is put back to water-bath heating.
It, can not be further out organic solvent environment, if for a long time in air after the stirring rod enters container stirring
Or touch water, then it must be cleaned and be reused with organic solvent.
The utility model has the advantages that the present invention is combined using heating stirring and cooling displacement, it is molten to significantly shorten complex compound gel
The time swap of agent promotes solvent displacement effect, and reduces the consumption of displacement solvent and the consumption of other energy resources, mentions
For the complex compound solvent method of replacing that one kind is high-efficient, effect is good and economizes on resources.
Detailed description of the invention
Fig. 1 is the concrete operations flow chart of the embodiment of the present invention 1.
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and examples, but is not limitation of the invention.
Embodiment 1:
Using strontium ferro-cobalt oxygen, citric acid complex gel as raw material, dehydrated alcohol is displacement solvent, is needed in technical process
Key instrument equipment: heat-collecting magnetic stirring water-bath 1,1 piece of magnetic stir bar, 1,100ml beaker, glass stirring rod 1
Branch.
Concrete operations process and phenomenon are as follows:
1) strontium ferro-cobalt oxygen, citric acid complex gel that total amount is 15ml are fitted into 100ml beaker, beaker is placed in 80 DEG C
Heat-collecting magnetic stirring water-bath in, magnetic stir bar is put into beaker, magnetic agitation wet gel, when wet gel liquid level no longer
At any time and heating stirring declines, that is, forms preliminary wet gel；
2) wet gel into step 1) is added at the dehydrated alcohol to beaker 85ml lower than 20 DEG C, continues magnetic agitation
30min can be continuously added dehydrated alcohol in the process, and liquid level is maintained to be higher than 60ml；
3) beaker is removed into water-bath, the dehydrated alcohol of wet gel upper layer remnants in step 2 is removed, nothing is rejoined
At water-ethanol to beaker 85ml, at room temperature, vertical direction is kept to stir gel colloidal along walls of beaker with glass bar, by beaker
Stirrable gel on wall stirs into dehydrated alcohol；A large amount of powders are formed in beaker at this time, are brown powder under acid condition,
It is bright yellow powder when pH > 6, anhydrous ethanol solvent displacement quickly occurs；
It is difficult to stir if 4) have residual gel in glass bar and walls of beaker and be hardened, needs to put back in 80 DEG C of water-bath
It is slightly hot, after gel softening can stir, beaker is taken out, continues to stir under room temperature, 1-2 times repeatedly；
5) it is added again into beaker at the dehydrated alcohol to 85ml of room temperature, continues to stir with small magneton in 80 DEG C of water-baths
Mix 30min；
6) beaker is taken out, dehydrated alcohol is drained, then the powder in beaker is taken out, is stored in the mill equipped with dehydrated alcohol
In sand mouth wide-mouth bottle.
Embodiment 2:
Using strontium ferro-cobalt oxygen, citric acid complex gel as raw material, acetone is displacement solvent, the master needed in technical process
Want instrument and equipment: heat-collecting magnetic stirring water-bath 1,1 piece of magnetic stir bar, 1,100ml beaker, glass stirring rod 1.
Concrete operations process and phenomenon are as follows:
1) strontium ferro-cobalt oxygen, citric acid complex gel that total amount is 15ml are fitted into 100ml beaker, beaker is placed in 15 DEG C
Heat-collecting magnetic stirring water-bath in, magnetic stir bar is put into beaker, magnetic agitation wet gel, when wet gel liquid level no longer
At any time and heating stirring declines, that is, forms preliminary wet gel；
2) wet gel into step 1) is added at the acetone to beaker 85ml lower than 20 DEG C, continues magnetic agitation 30min；
3) beaker is removed into water-bath, the acetone of wet gel upper layer remnants in step 2 is removed, rejoins acetone extremely
At beaker 85ml, at room temperature, with glass bar keep vertical direction along walls of beaker stir gel colloidal, by walls of beaker can
The gel of agitation stirs into acetone；A large amount of bright yellow powders are formed in beaker at this time, acetone solvent displacement quickly occurs；
4) acetone displacement coolant-temperature gage is lower, and gel has originally softened, and beaker is without putting back to water-bath in glass bar whipping process；
5) it is added at the acetone to 85ml lower than 20 DEG C again into beaker, continues to stir with small magneton in 15 DEG C of water-baths
Mix 30min；
6) beaker is taken out, acetone is drained, then the powder in beaker is taken out, is stored in the frosted mouth wide-mouth equipped with acetone
In bottle.
Claims (6)
1. a kind of efficient complex compound wet gel solvent method of replacing, which is characterized in that using heating stirring and cooling displacement phase
In conjunction with specifically comprising the following steps:
1) it observes the formation of wet gel: wet gel to be replaced being placed in container, container is placed under water bath with thermostatic control environment, magnetic force
Stir wet gel, when wet gel liquid level no longer at any time and heating stirring decline, that is, form preliminary wet gel；
2) organic solvent is added in the preliminary wet gel into step 1), continues magnetic agitation 30 minutes, forms new wet gel；
3) water bath is moved the containers out, the organic solvent of wet gel upper layer remnants new in step 2 is removed, is rejoined
Organic solvent；At room temperature, with stirring rod along chamber wall, vertical direction is kept to stir gel colloidal, by chamber wall can
The gel of agitation stirs into organic solvent, forms a large amount of powders in container at this time, and organic solvent displacement quickly occurs；
Be difficult to stir if 4) have residual gel on stirring rod or chamber wall and be hardened, container is put back to it is slightly hot in water-bath, to
After gel softening can stir, container is taken out, continues to stir under room temperature, 1-2 times repeatedly；
5) after gel is fully converted to the powder of fine uniform, container is taken out, organic solvent is drained, then by the powder in container
End, which is taken out, to be saved；
By above-mentioned steps, complex compound wet gel is successfully replaced, this replacement process total time-consuming is not more than 1 hour.
2. the method according to claim 1, wherein the temperature of the water bath with thermostatic control environment is 10 ~ 80 DEG C.
3. the method according to claim 1, wherein the organic solvent, surface tension is not more than 25 mN/
m。
4. according to the method described in claim 3, it is characterized in that, the organic solvent be dehydrated alcohol, acetone, methanol,
Normal propyl alcohol, n-butanol, methyl at least one of butanone, hexamethylene and normal heptane.
5. the method according to claim 1, wherein in the step 4), when the water-bath ring of organic solvent setting
Gel is remained when border temperature is lower than room temperature, when being stirred at room temperature originally to have softened, then is heated without putting back to container in water-bath.
6. the method according to claim 1, wherein the stirring rod enter container stirring after, can not again from
Organic solvent environment is opened, if in air or touching water for a long time, must be cleaned and be reused with organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710192411.9A CN106984062B (en) | 2017-03-28 | 2017-03-28 | A kind of efficient complex compound wet gel solvent method of replacing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710192411.9A CN106984062B (en) | 2017-03-28 | 2017-03-28 | A kind of efficient complex compound wet gel solvent method of replacing |
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| CN106984062A CN106984062A (en) | 2017-07-28 |
| CN106984062B true CN106984062B (en) | 2019-02-01 |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3164883D1 (en) * | 1980-09-11 | 1984-08-23 | Atomic Energy Authority Uk | Process for removing water from gel materials |
| CN1281498C (en) * | 2004-09-27 | 2006-10-25 | 大连理工大学 | Method of preparing nanometer magnesium oxide using uniform precipitation-supercritical carbon dioxide drying method |
| CN100377395C (en) * | 2006-01-19 | 2008-03-26 | 同济大学 | A kind of preparation method of nanocomposite lithium ion battery cathode material |
| CN101306842B (en) * | 2008-07-04 | 2010-12-08 | 华中科技大学 | A preparation method of ceramic cathode nanopowder for solid oxide fuel cell |
| KR101400721B1 (en) * | 2012-10-22 | 2014-05-29 | 지오스 에어로겔 리미티드 | Silica aerogel powder manufacturing system and manufacturing method using the same |
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