CN103131039A - Preparation method of nano-cellulose aerogel - Google Patents
Preparation method of nano-cellulose aerogel Download PDFInfo
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- CN103131039A CN103131039A CN2013100950599A CN201310095059A CN103131039A CN 103131039 A CN103131039 A CN 103131039A CN 2013100950599 A CN2013100950599 A CN 2013100950599A CN 201310095059 A CN201310095059 A CN 201310095059A CN 103131039 A CN103131039 A CN 103131039A
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Abstract
The invention discloses a preparation method of nano-cellulose aerogel and relates to the preparation method of the nano-cellulose aerogel. The preparation method aims at solving the problem of poor dispersion of the existing cellulose aerogel in an organic solvent. The preparation method comprises the following steps: 1) dissolving absorbent cotton in a sulfuric acid solution for acidolysis, centrifugalizing, and then washing a white sol precipitate with deionized water to be neutral; 2) adding the nano-cellulose sol precipitate into the organic solvent, uniformly stirring, and then placing into an ultrasonic cleaning instrument for ultrasonic dispersion; and 3) placing a nano-cellulose suspension at the temperature of minus 18-minus 25 DEG C for freezing, and then further placing into a freeze-drying machine for freeze-drying. The nano-cellulose aerogel prepared by the invention has obvious nano-microfibril and nano-porous structure and can be rapidly dispersed in the organic solvent, such as dimethylformamide, dimethylacetamide and the like, the particle size of dispersed cellulose is nano-scale, and the good dispersion is shown. The preparation method disclosed by the invention can be applied to catalyst carriers, adsorbents and other fields.
Description
Technical field
The present invention relates to a kind of preparation method of nano-cellulose aerogel.
Background technology
Organic aerogel is a kind of have vesicular structure, low solid content and even low-density organism solid-state material, and the characteristics of easy processing, good toughness are arranged than inorganic aerogels, is an important development direction of aerogel material research.Have a lot of hydroxyls based on fiber, the preparation process of gel can be very simple, need not linking agent, carry out physical crosslinking by hydrogen bond and can make aerogel, natural cellulose has wide material sources, renewable, easily degraded and the characteristic such as green non-pollution, prepares the cellulose aerogels material take Mierocrystalline cellulose as raw material and has caused the great interest of people.
But existing cellulose aerogels preparation technology is mainly to prepare cellulose aerogels after the cellosolve dissolving cellulos again, cellulose aerogels often adopts the supercritical drying drying process, preparation cycle is long, cost is high, complex process, and aerogel is in water or the dispersiveness in other solvents, is one of restrictive factor of using of aerogel material.
Summary of the invention
To the objective of the invention is to have the dispersed bad problem of cellulose aerogels now in order solving, and a kind of preparation method of nano-cellulose aerogel to be provided.
The preparation method of nano-cellulose aerogel of the present invention follows these steps to realize:
One, absorbent cotton being dissolved in massfraction is to obtain nano-cellulose suspension after acidolysis 3～6h in 55% sulphuric acid soln, nano-cellulose suspension obtains the leucosol precipitation with the centrifugal 8～15min of the rotating speed of 6000～10000r/min, use deionized water repeated washing leucosol to be precipitated to neutrality, obtain the nano cellulose sol precipitation;
Two, the volume ratio by nano cellulose sol precipitation and organic solvent is 1:(10～50) the nano cellulose sol precipitation of step 1 is joined in organic solvent, put into ultrasonic washing instrument with 45Hz ultra-sonic dispersion 5～10min after stirring 8～15min with 800r/min～1000r/min, obtain being dispersed in the nano-cellulose suspension in organic solvent;
Three, will be dispersed in freezing 20～26h at the temperature that nano-cellulose suspension in organic solvent is placed in-18～-25 ℃, obtain freezing gel, then putting into freeze drier is 16～24Pa in vacuum tightness, condenser temperature is lyophilize 10～14h under the condition of-45～-55 ℃, obtains the nano-cellulose aerogel;
Wherein the described organic solvent of step 2 is Isosorbide-5-Nitrae-dioxane, the trimethyl carbinol or dimethyl sulfoxide (DMSO).
The present invention makes nano-cellulose fully disperse to obtain freezing gel through freezing in organic solvent, formed metastable network structure in freezing gel inside, filled a large amount of organic solvents in network, and through after vacuum lyophilization, because organic solvent system exists weak liquid-gas interface and interfacial tension, so effect of liquid-gas interface and interfacial tension during existence overcomes solidification liquid in through the vacuum lyophilization process, prevent caving in of gel network, form the nano-cellulose aerogel with a large amount of pore structures.The nano-cellulose aerogel of the present invention's preparation has obvious nanometer micro-fibril and nano-porous structure, can rapid dispersion be nano-scale particle in the non-aqueous organic solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone, demonstrate good dispersiveness.Preparation method of the present invention is simple, easy handling, and cost is low, has a extensive future in fields such as support of the catalyst, sorbent materials.
Description of drawings
Fig. 1 is the transmission electron microscope figure of the nano-cellulose in embodiment one step 1 nano-cellulose suspension;
Fig. 2 is the particle size distribution figure of embodiment one step 1 nano-cellulose suspension;
Fig. 3 is the nano-cellulose aerogel scanning electron microscope diagram of embodiment one preparation;
Fig. 4 is the nano-cellulose aerogel scanning electron microscope diagram of embodiment two preparations;
Fig. 5 is the rapid dispersion granularity graph of nano-cellulose aerogel in dimethyl formamide of embodiment two preparations;
Fig. 6 is the nano-cellulose aerogel macro morphology figure of embodiment two preparations.
Embodiment
Embodiment one: the preparation method of present embodiment nano-cellulose aerogel follows these steps to implement:
One, absorbent cotton being dissolved in massfraction is to obtain nano-cellulose suspension after acidolysis 3～6h in 55% sulphuric acid soln, nano-cellulose suspension obtains the leucosol precipitation with the centrifugal 8～15min of the rotating speed of 6000～10000r/min, use deionized water repeated washing leucosol to be precipitated to neutrality, obtain the nano cellulose sol precipitation;
Two, the volume ratio by nano cellulose sol precipitation and organic solvent is 1:(10～50) the nano cellulose sol precipitation of step 1 is joined in organic solvent, put into ultrasonic washing instrument with 45Hz ultra-sonic dispersion 5～10min after stirring 8～15min with 800r/min～1000r/min, obtain being dispersed in the nano-cellulose suspension in organic solvent;
Three, will be dispersed in freezing 20～26h at the temperature that nano-cellulose suspension in organic solvent is placed in-18～-25 ℃, obtain freezing gel, then putting into freeze drier is 16～24Pa in vacuum tightness, condenser temperature is lyophilize 10～14h under the condition of-45～-55 ℃, obtains the nano-cellulose aerogel;
Wherein the described organic solvent of step 2 is Isosorbide-5-Nitrae-dioxane, the trimethyl carbinol or dimethyl sulfoxide (DMSO).
The nano-cellulose aerogel that present embodiment obtains disperses in organic solvent: be that 1:20～1:100 joins the nano-cellulose aerogel in organic dispersion solvent by nano-cellulose aerogel and organic dispersion solvent volume ratio, ultrasonic frequency be in the ultrasonic washing instrument of 45Hz with stirring velocity ultrasonic agitation 2～4min of 200r/min～1000r/min, obtain the nano-cellulose suspension organic solution of dispersing nanometer size; Wherein organic dispersion solvent is dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone.
Nano-cellulose in present embodiment not only can derive from absorbent cotton, can also use Microcrystalline Cellulose, wood pulp, straw pulp, bamboo pulp or agricultural stalk to replace absorbent cotton that nano-cellulose is provided.
The nano-cellulose aerogel that present embodiment obtains has obvious nanometer micro-fibril and nano-porous structure, can rapid dispersion be nano-scale particle in the non-aqueous organic solvents such as dimethyl formamide, N,N-DIMETHYLACETAMIDE or dimethyl pyrrolidone, demonstrate good dispersiveness.
Embodiment two: present embodiment is different from embodiment one, and to be step 1 be dissolved in the 100mL massfraction with 2.0g absorbent cotton is acidolysis in 55% sulphuric acid soln.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two, and to be step 1 be dissolved in massfraction with absorbent cotton is in 55% sulphuric acid soln, 50 ℃ of lower acidolysis.Other step and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is that step 1 nano-cellulose suspension is with the centrifugal 10min of the rotating speed of 8000r/min.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four, and be step 2 to be 1:20 by the volume ratio of nano cellulose sol precipitation and organic solvent join the nano cellulose sol precipitation of step 1 in organic solvent.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five is that organic solvent in step 2 is the trimethyl carbinol.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to five be in step 2 organic solvent for doping volume ratio in Isosorbide-5-Nitrae-dioxane lower than 10% water or in the trimethyl carbinol doping volume ratio lower than 10% water.Other step and parameter are identical with one of embodiment one to five.
Embodiment eight: present embodiment is different from one of embodiment one to seven is that step 3 nano-cellulose suspension is placed in freezing 24h at the temperature of-20 ℃.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight be the freezing gel of step 3 to put into freeze drier be 20Pa in vacuum tightness, condenser temperature is lyophilize under the condition of-50 ℃.Other step and parameter are identical with one of embodiment one to eight.
Embodiment one: the preparation method of the present embodiment nano-cellulose aerogel follows these steps to implement:
One, 2.0g absorbent cotton being dissolved in the 100mL massfraction is in 55% sulphuric acid soln, obtain nano-cellulose suspension after 50 ℃ of lower acidolysis 4h, nano-cellulose suspension obtains the leucosol precipitation with the centrifugal 10min of the rotating speed of 8000r/min, use deionized water repeated washing leucosol to be precipitated to neutrality, obtain the nano cellulose sol precipitation;
Two, being 1:20 by the volume ratio of nano cellulose sol precipitation and organic solvent joins the nano cellulose sol precipitation of step 1 in organic solvent, put into ultrasonic washing instrument with 45Hz ultra-sonic dispersion 5min after stirring 10min with 800r/min, obtain being dispersed in the nano-cellulose suspension in organic solvent;
Three, will be dispersed in freezing 24h at the temperature that nano-cellulose suspension in organic solvent is placed in-20 ℃, obtain freezing gel, then putting into freeze drier is 20Pa in vacuum tightness, and condenser temperature is lyophilize 12h under the condition of-50 ℃, obtains the nano-cellulose aerogel;
Wherein the described organic solvent of step 2 is the trimethyl carbinol.
The transmission electron microscope figure of the nano-cellulose in the present embodiment step 1 nano-cellulose suspension as shown in Figure 1, nano-cellulose suspension particle size distribution figure as shown in Figure 2, the Mierocrystalline cellulose granularity is nano level;
The scanning electron microscope diagram of the nano-cellulose aerogel that the present embodiment obtains as shown in Figure 3, the nano-cellulose aerogel has obvious nanometer micro-fibril and nano-porous structure.
The nano-cellulose aerogel that the present embodiment is obtained disperses in organic solvent: be that 1:20 joins the nano-cellulose aerogel in dimethyl formamide by nano-cellulose aerogel and organic dispersion solvent dimethyl formamide volume ratio, be with the stirring velocity ultrasonic agitation 2min of 800r/min in the ultrasonic washing instrument of 45Hz in ultrasonic frequency, obtain the nano-cellulose suspension organic solution of dispersing nanometer size, demonstrate the good dispersiveness of nano-cellulose aerogel.
Embodiment two: the preparation method of the present embodiment nano-cellulose aerogel follows these steps to implement:
One, 2.0g absorbent cotton being dissolved in the 100mL massfraction is in 55% sulphuric acid soln, obtain nano-cellulose suspension after 50 ℃ of lower acidolysis 4h, nano-cellulose suspension obtains the leucosol precipitation with the centrifugal 10min of the rotating speed of 8000r/min, use deionized water repeated washing leucosol to be precipitated to neutrality, obtain the nano cellulose sol precipitation;
Two, being 1:20 by the volume ratio of nano cellulose sol precipitation and organic solvent joins the nano cellulose sol precipitation of step 1 in organic solvent, put into ultrasonic washing instrument with 45Hz ultra-sonic dispersion 5min after stirring 10min with 800r/min, obtain being dispersed in the nano-cellulose suspension in organic solvent;
Three, will be dispersed in freezing 24h at the temperature that nano-cellulose suspension in organic solvent is placed in-20 ℃, obtain freezing gel, then putting into freeze drier is 20Pa in vacuum tightness, and condenser temperature is lyophilize 12h under the condition of-50 ℃, obtains the nano-cellulose aerogel;
Wherein the described organic solvent of step 2 is Isosorbide-5-Nitrae-dioxane.
The scanning electron microscope diagram of the nano-cellulose aerogel that the present embodiment obtains as shown in Figure 4, the nano-cellulose aerogel has obvious nanometer micro-fibril and nano-porous structure, nano-cellulose aerogel macro morphology figure as shown in Figure 6.
the nano-cellulose aerogel that the present embodiment is obtained disperses in organic solvent: be that 1:20 joins the nano-cellulose aerogel in dimethyl formamide by nano-cellulose aerogel and organic dispersion solvent dimethyl formamide volume ratio, be with the stirring velocity ultrasonic agitation 2min of 800r/min in the ultrasonic washing instrument of 45Hz in ultrasonic frequency, obtain the nano-cellulose suspension organic solution of dispersing nanometer size, the rapid dispersion granularity graph of nano-cellulose aerogel in dimethyl formamide as shown in Figure 5, the Mierocrystalline cellulose granularity of scheming thus to disperse as can be known is nano level, even particle size distribution, demonstrate the good dispersiveness of nano-cellulose aerogel.
Claims (9)
1. the preparation method of a nano-cellulose aerogel is characterized in that the preparation method of nano-cellulose aerogel follows these steps to realize:
One, absorbent cotton being dissolved in massfraction is to obtain nano-cellulose suspension after acidolysis 3～6h in 55% sulphuric acid soln, nano-cellulose suspension obtains the leucosol precipitation with the centrifugal 8～15min of the rotating speed of 6000～10000r/min, use deionized water repeated washing leucosol to be precipitated to neutrality, obtain the nano cellulose sol precipitation;
Two, the volume ratio by nano cellulose sol precipitation and organic solvent is 1:(10～50) the nano cellulose sol precipitation of step 1 is joined in organic solvent, put into ultrasonic washing instrument with 45Hz ultra-sonic dispersion 5～10min after stirring 8～15min with 800r/min～1000r/min, obtain being dispersed in the nano-cellulose suspension in organic solvent;
Three, will be dispersed in freezing 20～26h at the temperature that nano-cellulose suspension in organic solvent is placed in-18～-25 ℃, obtain freezing gel, then putting into freeze drier is 16～24Pa in vacuum tightness, condenser temperature is lyophilize 10～14h under the condition of-45～-55 ℃, obtains the nano-cellulose aerogel;
Wherein the described organic solvent of step 2 is Isosorbide-5-Nitrae-dioxane, the trimethyl carbinol or dimethyl sulfoxide (DMSO).
2. the preparation method of a kind of nano-cellulose aerogel according to claim 1 is characterized in that it is acidolysis in 55% sulphuric acid soln that step 1 is dissolved in the 100mL massfraction with 2.0g absorbent cotton.
3. the preparation method of a kind of nano-cellulose aerogel according to claim 1 and 2 is characterized in that it is in 55% sulphuric acid soln, 50 ℃ of lower acidolysis that step 1 is dissolved in massfraction with absorbent cotton.
4. the preparation method of a kind of nano-cellulose aerogel according to claim 1, is characterized in that step 1 nano-cellulose suspension is with the centrifugal 10min of the rotating speed of 8000r/min.
5. the preparation method of a kind of nano-cellulose aerogel according to claim 1 is characterized in that step 2 is 1:20 by the volume ratio of nano cellulose sol precipitation and organic solvent the nano cellulose sol precipitation of step 1 is joined in organic solvent.
6. the preparation method of a kind of nano-cellulose aerogel according to claim 1, is characterized in that the organic solvent in step 2 is the trimethyl carbinol.
7. the preparation method of a kind of nano-cellulose aerogel according to claim 6, it is characterized in that in step 2 organic solvent for doping volume ratio in Isosorbide-5-Nitrae-dioxane lower than 10% water or in the trimethyl carbinol doping volume ratio lower than 10% water.
8. the preparation method of a kind of nano-cellulose aerogel according to claim 1 is characterized in that step 3 nano-cellulose suspension is placed in freezing 24h at the temperature of-20 ℃.
9. the preparation method of a kind of nano-cellulose aerogel according to claim 1, is characterized in that it is 20Pa in vacuum tightness that the freezing gel of step 3 is put into freeze drier, and condenser temperature is lyophilize under the condition of-50 ℃.
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Cited By (8)
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| CN105131328A (en) * | 2015-09-23 | 2015-12-09 | 黑龙江大学 | Preparation method for polymer aerogel |
| CN105625077A (en) * | 2016-03-27 | 2016-06-01 | 张耀忠 | Preparation method for nano-cellulose |
| CN107722338A (en) * | 2017-10-31 | 2018-02-23 | 天津科技大学 | The preparation method and nano-cellulose aerogel of a kind of nano-cellulose aerogel |
| WO2018106190A1 (en) * | 2016-12-09 | 2018-06-14 | National University Of Singapore | A polysaccharide aerogel |
| CN111974356A (en) * | 2020-07-24 | 2020-11-24 | 华南理工大学 | Composite aerogel type cigarette filter tip material and preparation method and application thereof |
| CN112619569A (en) * | 2021-01-20 | 2021-04-09 | 国际竹藤中心 | Bamboo-based directional aerogel and preparation method thereof |
| CN113716896A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Silica aerogel-based flame-retardant composite shaping phase-change material, and preparation and application thereof |
| CN117089093A (en) * | 2023-02-10 | 2023-11-21 | 河源市万利科技有限公司 | Environment-friendly furniture decorative film and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131328A (en) * | 2015-09-23 | 2015-12-09 | 黑龙江大学 | Preparation method for polymer aerogel |
| CN105625077A (en) * | 2016-03-27 | 2016-06-01 | 张耀忠 | Preparation method for nano-cellulose |
| WO2018106190A1 (en) * | 2016-12-09 | 2018-06-14 | National University Of Singapore | A polysaccharide aerogel |
| CN110088187A (en) * | 2016-12-09 | 2019-08-02 | 新加坡国立大学 | Polysaccharide aeroge |
| US11103845B2 (en) | 2016-12-09 | 2021-08-31 | National University Of Singapore | Polysaccharide aerogel |
| CN110088187B (en) * | 2016-12-09 | 2021-10-22 | 新加坡国立大学 | Polysaccharide aerogel |
| CN107722338A (en) * | 2017-10-31 | 2018-02-23 | 天津科技大学 | The preparation method and nano-cellulose aerogel of a kind of nano-cellulose aerogel |
| CN113716896A (en) * | 2020-05-25 | 2021-11-30 | 中国科学院大连化学物理研究所 | Silica aerogel-based flame-retardant composite shaping phase-change material, and preparation and application thereof |
| CN111974356A (en) * | 2020-07-24 | 2020-11-24 | 华南理工大学 | Composite aerogel type cigarette filter tip material and preparation method and application thereof |
| CN111974356B (en) * | 2020-07-24 | 2021-10-22 | 华南理工大学 | Composite aerogel type cigarette filter tip material and preparation method and application thereof |
| CN112619569A (en) * | 2021-01-20 | 2021-04-09 | 国际竹藤中心 | Bamboo-based directional aerogel and preparation method thereof |
| CN117089093A (en) * | 2023-02-10 | 2023-11-21 | 河源市万利科技有限公司 | Environment-friendly furniture decorative film and preparation method thereof |
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Application publication date: 20130605 |