CN103319746A - Preparation method for spherical cellulose aerogel - Google Patents
Preparation method for spherical cellulose aerogel Download PDFInfo
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- CN103319746A CN103319746A CN2013102942332A CN201310294233A CN103319746A CN 103319746 A CN103319746 A CN 103319746A CN 2013102942332 A CN2013102942332 A CN 2013102942332A CN 201310294233 A CN201310294233 A CN 201310294233A CN 103319746 A CN103319746 A CN 103319746A
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Abstract
The invention provides a preparation method for a spherical cellulose aerogel, which relates to a preparation method for an aerogel. The objective of the invention is to overcome the problems that the phenomena of structure collapse and volume contraction of a conventional cellulose aerogel frequently occur and the specific surface area of an obtained aerogel is small. The method comprises the following steps: 1, putting vegetable fiber in a mixed solution of urea and NaOH and carrying out stirring after refrigeration for formation of a solution so as to obtain a vegetable fiber/alkaline urea solution; 2, mixing trichloromethane with ethyl acetate and then adding glacial acetic acid so as to obtain an organic solution; 3, titrating the vegetable fiber/alkaline urea solution into the organic solution of glacial acetic acid and carrying out ageing so as to obtain a gel; 4, putting the gel into a glacial acetic acid solution for solidification; and 5, replacing a hydrogel successively with absolute ethyl alcohol and tert-butyl alcohol and carrying out refrigeration and freeze-drying so as to obtain the aerogel. According to the invention, the phenomena of structure collapse and volume contraction of an aerogel in the process of drying are overcome, and the prepared cellulose aerogel has low density and a specific surface area of more than 240 m<2>/g.
Description
Technical field
The present invention relates to a kind of preparation method of aerogel.
Background technology
Aerogel is to be gathered into the nanoporous network structure mutually by colloidal particle or high-polymer molecular, and is full of a kind of high dispersive solid-state material of gaseous state dispersion medium in hole.Common preparation method mainly contains sol-gel method and solution regenerative method etc.Compare with solution regenerative method, the cost of sol-gel method is than higher.In addition, in the preparation process of aerogel, understand phenomenons such as recurring structure subsides, volumetric shrinkage usually, make the structure of aerogel be subjected to serious destruction, and then influence its high performance performance.
Summary of the invention
The objective of the invention is to be prone to the phenomenon of structural collapse and volumetric shrinkage in order to solve existing cellulose aerogels, and the low problem of the specific surface area of the aerogel that obtains, and a kind of preparation method of ball shaped cellulose aerogel is provided.
The preparation method of ball shaped cellulose aerogel of the present invention realizes according to the following steps:
One, the vegetable fibre that takes by weighing 1.00～3.00g is put into the mixing solutions of urea and NaOH, obtain mixed system, mixed system is placed under-18～-20 ℃ the temperature and takes out behind freezing 2～4h, at room temperature thaw, stir into solution then and obtain vegetable fibre/alkali urea solution;
Two, the trichloromethane of 100～200mL and the ethyl acetate of 100～200mL are mixed, and then the Glacial acetic acid that adds 20～40mL obtains the organic solution of Glacial acetic acid;
Three, the vegetable fibre that step 1 is obtained with titration apparatus/alkali urea solution is titrated in the organic solution of Glacial acetic acid of step 2, forms the pearl body, again the pearl body is placed the aging 5～15min of organic solution of Glacial acetic acid of step 2 after, obtain white spherical gel;
Four, the white spherical gel that step 3 is obtained is put into glacial acetic acid solution and is solidified 22～26h, is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, per 10～13h changes a dehydrated alcohol, replace altogether 4～5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, per 10～13h changes a trimethyl carbinol, replace altogether 4～5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 22～26h under-16～-20 ℃ temperature, and the vacuum lyophilization through 22～26h obtains the ball shaped cellulose aerogel again.
Step 3 of the present invention is titrated to vegetable fibre/alkali urea solution in the organic solution of Glacial acetic acid by adopting the glue head dropper of different sizes, prepares the ball shaped cellulose aerogel of different size.
The method that the present invention adopts solution regenerative method to combine with the titration suspension method with the solvent of the trimethyl carbinol as gel, has been prepared the ball shaped cellulose aerogel of low density, high porosity by lyophilize.The present invention is by adopting solvent exchange, with the solvent of the little trimethyl carbinol of volume change when freezing as the ball shaped cellulose aerogel, overcome phenomenons such as aerogel recurring structure in drying process subsides, volumetric shrinkage, kept its original constitutional features.
Adopt the ball shaped cellulose aerogel of the inventive method preparation, easy and simple to handle, cost is low, and the ball shaped cellulose aerogel of preparing has low density, and specific surface area can reach 240m
2G
-1More than, porosity is higher.The present invention is mainly used in catalytic field and adsorbing domain.
Description of drawings
The macro morphology figure of the ball shaped cellulose aerogel that Fig. 1 obtains for embodiment one;
The Fourier transform infrared spectrogram of the ball shaped cellulose aerogel that Fig. 2 obtains for embodiment one, wherein a represents the infrared line of bamboo fibers, b represents the infrared line of ball shaped cellulose aerogel;
Fig. 3 is the surface topography scanning electron microscope diagram of the ball shaped cellulose aerogel of embodiment one preparation;
Fig. 4 is the cross-section morphology scanning electron microscope diagram of the ball shaped cellulose aerogel of embodiment one preparation.
Embodiment
Embodiment one: the preparation method of present embodiment ball shaped cellulose aerogel realizes according to the following steps:
One, the vegetable fibre that takes by weighing 1.00～3.00g is put into the mixing solutions of urea and NaOH, obtain mixed system, mixed system is placed under-18～-20 ℃ the temperature and takes out behind freezing 2～4h, at room temperature thaw, stir into solution then and obtain vegetable fibre/alkali urea solution;
Two, the trichloromethane of 100～200mL and the ethyl acetate of 100～200mL are mixed, and then the Glacial acetic acid that adds 20～40mL obtains the organic solution of Glacial acetic acid;
Three, the vegetable fibre that step 1 is obtained with titration apparatus/alkali urea solution is titrated in the organic solution of Glacial acetic acid of step 2, forms the pearl body, again the pearl body is placed the aging 5～15min of organic solution of Glacial acetic acid of step 2 after, obtain white spherical gel;
Four, the white spherical gel that step 3 is obtained is put into glacial acetic acid solution and is solidified 22～26h, is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, per 10～13h changes a dehydrated alcohol, replace altogether 4～5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, per 10～13h changes a trimethyl carbinol, replace altogether 4～5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 22～26h under-16～-20 ℃ temperature, and the vacuum lyophilization through 22～26h obtains the ball shaped cellulose aerogel again.
The present embodiment step 1 is freezing under-16～-20 ℃ temperature in freezing and step 5 under-18～-20 ℃ the temperature all to be freezing in refrigerator, and the stirring in the step 1 is to use magnetic stirring apparatus to stir.Step 5 then cements out the ethanol in the cellulose gel by the trimethyl carbinol.
Embodiment two: what present embodiment and embodiment one were different is that vegetable fibre is bamboo fibers, lumber fibre or stalk fibre.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different with embodiment one or two is that the mass ratio of NaOH in the mixing solutions of step 1 urea and NaOH, urea and water is 7: 12: 81.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different with one of embodiment one to three is that the described solution that stirs into of step 1 is that speed with 400～800r/min stirs.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different with one of embodiment one to four is that titration apparatus in the step 3 is glue head dropper or needle tubing.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: that present embodiment is different with one of embodiment one to five is step 5 ball shaped cellulose alcogel freezing 24h under-18 ℃ temperature.Other step and parameter are identical with one of embodiment one to five.
Embodiment one: the preparation method of present embodiment ball shaped cellulose aerogel realizes according to the following steps:
One, the bamboo fibers that takes by weighing 2.00g is put into the urea of 100mL and the mixing solutions of NaOH, obtain mixed system, mixed system is placed under-18 ℃ the temperature and takes out behind the freezing 3h, at room temperature thaw, under magnetic stirring apparatus, stir into solution with the speed of 600r/min then and obtain bamboo fibers/alkali urea solution;
Two, the trichloromethane of 150mL and the ethyl acetate of 150mL are mixed, and then add the organic solution that the 30mL Glacial acetic acid obtains Glacial acetic acid;
Three, be in the organic solution of bamboo fibers/alkali urea solution that the glue head dropper of 2.320mm obtains step 1 Glacial acetic acid of being titrated to step 2 with the 2mL bore, form the pearl body, after again the pearl body being placed the aging 10min of organic solution of Glacial acetic acid of step 2, obtain white spherical gel;
Four, to put into mass concentration be that 1% Glacial acetic acid solidifies 24h to the white spherical gel that step 3 is obtained, and is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, every 12h changes a dehydrated alcohol, replace altogether 5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, every 12h changes a trimethyl carbinol, replace altogether 5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 24h under-18 ℃ temperature, and the vacuum lyophilization through 24h obtains the ball shaped cellulose aerogel again.
Wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixing solutions of step 1 urea and NaOH.
The macro morphology figure of the ball shaped cellulose aerogel that present embodiment obtains as shown in Figure 1, Fig. 2 is the Fourier transform infrared spectrogram of ball shaped cellulose aerogel, Fig. 3 is the surface topography scanning electron microscope diagram of ball shaped cellulose aerogel, and Fig. 4 is the cross-section morphology scanning electron microscope diagram of ball shaped cellulose aerogel.
Embodiment two: the preparation method of present embodiment ball shaped cellulose aerogel realizes according to the following steps:
One, the bamboo fibers that takes by weighing 2.00g is put into the urea of 100mL and the mixing solutions of NaOH, obtain mixed system, mixed system is placed under-18 ℃ the temperature and takes out behind the freezing 3h, at room temperature thaw, under magnetic stirring apparatus, stir into solution with the speed of 600r/min then and obtain bamboo fibers/alkali urea solution;
Two, the trichloromethane of 150mL and the ethyl acetate of 150mL are mixed, and then add the organic solution that the 30mL Glacial acetic acid obtains Glacial acetic acid;
Three, the bamboo fibers that step 1 is obtained with needle tubing/alkali urea solution is titrated in the organic solution of Glacial acetic acid of step 2, forms the pearl body, again the pearl body is placed the aging 10min of organic solution of Glacial acetic acid of step 2 after, obtain white spherical gel;
Four, to put into mass concentration be that 1% Glacial acetic acid solidifies 24h to the white spherical gel that step 3 is obtained, and is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, every 12h changes a dehydrated alcohol, replace altogether 5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, every 12h changes a trimethyl carbinol, replace altogether 5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 24h under-18 ℃ temperature, and the vacuum lyophilization through 24h obtains the ball shaped cellulose aerogel again.
Wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixing solutions of step 1 urea and NaOH.The syringe needle diameter of the described needle tubing of step 3 is 0.130mm.
Embodiment three: the preparation method of present embodiment ball shaped cellulose aerogel realizes according to the following steps:
One, the bamboo fibers that takes by weighing 2.00g is put into the urea of 100mL and the mixing solutions of NaOH, obtain mixed system, mixed system is placed under-18 ℃ the temperature and takes out behind the freezing 3h, at room temperature thaw, under magnetic stirring apparatus, stir into solution with the speed of 600r/min then and obtain bamboo fibers/alkali urea solution;
Two, the trichloromethane of 150mL and the ethyl acetate of 150mL are mixed, and then add the organic solution that the 30mL Glacial acetic acid obtains Glacial acetic acid;
Three, the bamboo fibers that step 1 is obtained with glue head dropper/alkali urea solution is titrated in the organic solution of Glacial acetic acid of step 2, forms the pearl body, again the pearl body is placed the aging 10min of organic solution of Glacial acetic acid of step 2 after, obtain white spherical gel;
Four, to put into mass concentration be that 1% Glacial acetic acid solidifies 24h to the white spherical gel that step 3 is obtained, and is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, every 12h changes a dehydrated alcohol, replace altogether 5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, every 12h changes a trimethyl carbinol, replace altogether 5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 24h under-18 ℃ temperature, and the vacuum lyophilization through 24h obtains the ball shaped cellulose aerogel again.
Wherein the mass ratio of NaOH, urea and water is 7: 12: 81 in the mixing solutions of step 1 urea and NaOH.The described glue head of step 3 dropper is that the dropper mouth with the glue head dropper of 5mL is cut into the glue head dropper that bore is 5.085mm.
The characterization data of the ball shaped cellulose aerogel that embodiment one, embodiment two and embodiment three obtain sees Table 1;
Table 1
Adopt the density of the ball shaped cellulose aerogel that the present invention prepares lower as can be known by table 1, have higher specific surface area simultaneously.
Claims (6)
1. the preparation method of a ball shaped cellulose aerogel is characterized in that the preparation method of ball shaped cellulose aerogel realizes according to the following steps:
One, the vegetable fibre that takes by weighing 1.00～3.00g is put into the mixing solutions of urea and NaOH, obtain mixed system, mixed system is placed under-18～-20 ℃ the temperature and takes out behind freezing 2～4h, at room temperature thaw, stir into solution then and obtain vegetable fibre/alkali urea solution;
Two, the trichloromethane of 100～200mL and the ethyl acetate of 100～200mL are mixed, and then the Glacial acetic acid that adds 20～40mL obtains the organic solution of Glacial acetic acid;
Three, the vegetable fibre that step 1 is obtained with titration apparatus/alkali urea solution is titrated in the organic solution of Glacial acetic acid of step 2, forms the pearl body, again the pearl body is placed the aging 5～15min of organic solution of Glacial acetic acid of step 2 after, obtain white spherical gel;
Four, the white spherical gel that step 3 is obtained is put into glacial acetic acid solution and is solidified 22～26h, is washed till neutrality with distilled water, obtains the spherical fiber hydrogel;
Five, the spherical fiber hydrogel that step 4 is obtained is dipped into and carries out solvent exchange in the dehydrated alcohol, per 10～13h changes a dehydrated alcohol, replace altogether 4～5 times, from dehydrated alcohol, take out the spherical fiber hydrogel, with the trimethyl carbinol spherical fiber hydrogel is carried out the dehydrated alcohol displacement again, per 10～13h changes a trimethyl carbinol, replace altogether 4～5 times, obtain the ball shaped cellulose alcogel, the ball shaped cellulose alcogel is freezing 22～26h under-16～-20 ℃ temperature, and the vacuum lyophilization through 22～26h obtains the ball shaped cellulose aerogel again.
2. the preparation method of a kind of ball shaped cellulose aerogel according to claim 1 is characterized in that vegetable fibre is bamboo fibers, lumber fibre or stalk fibre.
3. the preparation method of a kind of ball shaped cellulose aerogel according to claim 1 is characterized in that the mass ratio of NaOH, urea and water in the mixing solutions of step 1 urea and NaOH is 7: 12: 81.
4. the preparation method of a kind of ball shaped cellulose aerogel according to claim 1 is characterized in that the described solution that stirs into of step 1 is that speed with 400～800r/min stirs.
5. the preparation method of a kind of ball shaped cellulose aerogel according to claim 1 is characterized in that the titration apparatus in the step 3 is glue head dropper or needle tubing.
6. the preparation method of a kind of ball shaped cellulose aerogel according to claim 1 is characterized in that step 5 ball shaped cellulose alcogel freezing 24h under-18 ℃ temperature.
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Cited By (7)
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| CN103570967A (en) * | 2013-10-17 | 2014-02-12 | 东北林业大学 | Method for preparing regenerated cellulose spherical aerogel modified through carboxylation |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
| CN104017235A (en) * | 2014-06-23 | 2014-09-03 | 东北林业大学 | Preparation method of blocky regenerated cellulose composite phase change energy storage aerogel |
| CN105664948A (en) * | 2016-01-06 | 2016-06-15 | 江苏大学 | Preparation method and application of nickel-based dried gel catalyst |
| CN108359056A (en) * | 2018-03-06 | 2018-08-03 | 中国科学院理化技术研究所 | A kind of self-healing hydrogel and its preparation method and application of cellulose-dopamine-polymer composites |
| CN109762205A (en) * | 2019-01-04 | 2019-05-17 | 江苏泛亚微透科技股份有限公司 | A kind of structure-controllable pure cellulose aeroge and preparation method thereof |
| CN109821484A (en) * | 2019-03-27 | 2019-05-31 | 中国科学院化学研究所 | A kind of dipeptides aeroge and the preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103570967A (en) * | 2013-10-17 | 2014-02-12 | 东北林业大学 | Method for preparing regenerated cellulose spherical aerogel modified through carboxylation |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
| CN103756006B (en) * | 2014-01-20 | 2016-01-20 | 东北林业大学 | A kind of preparation method of nanofibrils cellulose aerogel of ultralight, hydrophobic, high oil absorbency |
| CN104017235A (en) * | 2014-06-23 | 2014-09-03 | 东北林业大学 | Preparation method of blocky regenerated cellulose composite phase change energy storage aerogel |
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| CN105664948B (en) * | 2016-01-06 | 2018-08-10 | 江苏大学 | A kind of preparation method and application of Ni-based xerogel catalyst |
| CN108359056A (en) * | 2018-03-06 | 2018-08-03 | 中国科学院理化技术研究所 | A kind of self-healing hydrogel and its preparation method and application of cellulose-dopamine-polymer composites |
| CN108359056B (en) * | 2018-03-06 | 2020-04-24 | 中国科学院理化技术研究所 | Self-healing hydrogel of cellulose-dopamine-polymer composite material and preparation method and application thereof |
| CN109762205A (en) * | 2019-01-04 | 2019-05-17 | 江苏泛亚微透科技股份有限公司 | A kind of structure-controllable pure cellulose aeroge and preparation method thereof |
| CN109821484A (en) * | 2019-03-27 | 2019-05-31 | 中国科学院化学研究所 | A kind of dipeptides aeroge and the preparation method and application thereof |
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