CN103146017A - Method for preparing aerogel by quickly dissolving lignocellulose - Google Patents
Method for preparing aerogel by quickly dissolving lignocellulose Download PDFInfo
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- CN103146017A CN103146017A CN2013100707802A CN201310070780A CN103146017A CN 103146017 A CN103146017 A CN 103146017A CN 2013100707802 A CN2013100707802 A CN 2013100707802A CN 201310070780 A CN201310070780 A CN 201310070780A CN 103146017 A CN103146017 A CN 103146017A
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Abstract
The invention discloses a method for preparing aerogel by quickly dissolving lignocellulose, and relates to a method for preparing the aerogel. The problems that the existing lignocellulose is low in dissolution efficiency and cannot meet market demand are solved. The method comprises the following steps of: (1) using natural lignocellulose as a solute and using ion liquid as a solvent; (2) quickly dissolving lignocellulose to form a brown solution; (3) cooling the solution and pouring anti-solvent into the solution for precipitating and gelating the lignocellulose solution; (4) changing the anti-solvent for several times and totally replacing the ion liquid to form lignocellulose hydrogel; and (5) drying and processing the hydrogel to obtain an aerogel material. According to the method, the ion liquid can be recovered and recycled, and the prepared lignin aerogel has an excellent porous structure and has certain mechanical strength and is complete in form, so that the efficient utilization of low-quality wood resources is increased.
Description
Technical field
The present invention relates to a kind of method for preparing aerogel.
Background technology
Environmental pollution along with quick disappearance and the petroleum chemicals consumption of petroleum resources causes begins to make the whole world to begin to pay close attention to reproducible Wooden Biomass resource as the alternate resources that can replace the petrochemical complex resource.The lignocellulose biomass resource comprises Wood waste, papermaking residue, the non-edible part of farm crop, resource crop etc.Lignocellulose is the abundantest biomass of content on the earth, is present in widely in woody, herbaceous plant.Its main component is the polymers such as Mierocrystalline cellulose, hemicellulose and xylogen, and Mierocrystalline cellulose is wrapped in by hemicellulose, and skin is again by the tight embedding of xylogen, and mutually combining becomes firm cell walls.Wherein Mierocrystalline cellulose is about 35 – 50%, hemicellulose is 20 – 35%, and xylogen is about 5 – 30%.
But in present " biorefining " concept, think and only have Mierocrystalline cellulose and hemicellulose to be developed as widely chemical and novel material.And the most complicated xylogen of structure is take phenylpropyl alcohol alkane as unit, connects by ehter bond and C-C the amorphous high polymer that forms.This macromolecular compound contains aromatic base, phenolic hydroxyl group alcoholic extract hydroxyl group, carboxyl, methoxyl group, carboxyl, conjugated double bond isoreactivity group, do not obtain at present the utilization of high value, due to the material that lacks suitable technology and convert it into high value, most xylogen is used to burn.Should comprise in the new technology of continual exploitation all components in lignocellulose (comprising xylogen) is converted into type material, lignocellulose aerogel for example is to cater to better all challenges of environment, economy, science and technology.With traditional inorganic aerogels (SiO
2, TiO
2And Fe
2O
3) compare, the Polymer Gas gel has higher physical strength, can bear higher surging force.Simultaneously, the lignocellulose aerogel also has the potentiality that become fexible conductor, because it can form crosslinked carbon aerogels by carbonization.For synthetic lignocellulose aerogel, the challenge that stands in the breach is dissolved in lignocellulose in working medium exactly.Therefore, we have used a class biomacromolecule to be had the novel dissolvent of high resolution--ionic liquid (ILs).Particularly AMImCl (1-allyl group-Methylimidazole villaumite 1-allyl-3-methylimidazoliumchloride) is as the working medium of suitable dissolving cellulos and xylogen; can destroy the intermolecular hydrogen bond of each component of lignocellulose; disintegrate xylogen and hemicellulose to cellulosic provide protection; destroy cellulosic crystalline texture; each component macromole is separated from each other, lignocellulose is dissolved fully.But present dissolving technology needs the time of 4h at least, usually to lengthen mechanical stirring fast, could completely lignocellulose be dissolved, and in the process of preparation lignocellulose aerogel, also need the frozen-thaw process by repeatedly to make polymer generation physical crosslinking, this process length consuming time, step are more complicated, production lignocellulose aerogel material that can not be quick, a large amount of.
Summary of the invention
The present invention will solve that in existing lignocellulose aerogel material preparation method, dissolution rate is slow, preparation cycle is long, the problem that can not meet the need of market, and provide a kind of quick dissolving lignocellulose to prepare the method for aerogel.
A kind of quick dissolving lignocellulose prepares the method for aerogel, specifically carries out according to the following steps:
One, get lignocellulosic material after washing removal of impurities, drying and pulverizing, cross 40～200 eye mesh screens, then after the ratio that is 0.1～20:100 in mass ratio with lignocellulosic material and ionic liquid is mixed, after being heated to 150～200 ℃ of stirring 5～20min, get the wood fibre cellulose solution; Two, mentioned solution is cooling; Three, add non-solvent in the cooled wood fibre cellulose solution of step 2, get gel; Four, the gel that step 3 is obtained namely gets the lignocellulose aerogel after critical point drying, supercritical drying or lyophilize.
The present invention has following beneficial effect:
One, lignocellulose aerogel dissolved efficiency in ionic liquid of preparing of existing method is lower, at least need the above dissolution time of 4h, and lignocellulose aerogel dissolution time in ionic liquid of preparation method provided by the invention is no more than 20min, demand that can satisfying the market;
Two, preparation method provided by the invention, preparation process is simple, does not need expensive device, extensive, the with low cost and environment-friendly and green of raw material sources, the preparation method is safe, can not bring pollution to environment;
Three, the lignocellulose aerogel of the inventive method preparation can directly precipitate gelling in non-solvent, does not need freeze thawing treatment repeatedly;
Four, preparation method's process provided by the invention is simple, and technique is easily controlled.
Five, xylon gas's gel of preparation method's preparation provided by the invention is of many uses, can be used for sound insulation, thermal insulation, oil suction, wrapping material, energy storage material, load nano particle, carbon aerogels presoma etc., belongs to high value added product, has wide application prospects.
In step 1 of the present invention, temperature must be higher than the second-order transition temperature of xylogen, although the difference of raw material wood element kind and water ratio can affect second-order transition temperature, Heating temperature is not less than 150 ℃.Because the ionic liquid that uses easily decomposes at higher temperature, the temperature of heating can not be higher than 200 ℃, and the time of heating can not surpass 20min.
Description of drawings
Fig. 1 is the SEM figure of the test 1 mountain jute lignocellulose aerogel that makes;
Fig. 2 is the SEM figure of the test 2 maize peel lignocellulose aerogels that make;
Fig. 3 is the SEM figure of the test 3 maize straw lignocellulose aerogels that make;
Fig. 4 is the SEM figure of the wooden cellulose aerogels of China fir of test 4 preparations that make;
Fig. 5 is the SEM figure of the test 5 bamboo lignocellulose aerogels that make.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of quick dissolving lignocellulose of present embodiment prepares the method for aerogel, specifically carries out according to the following steps:
One, get lignocellulosic material after washing removal of impurities, drying and pulverizing, cross 40～200 eye mesh screens, then after the ratio that is 0.1～20:100 in mass ratio with lignocellulosic material and ionic liquid is mixed, after being heated to 150～200 ℃ of stirring 5～20min, get the wood fibre cellulose solution; Two, mentioned solution is cooling; Three, add non-solvent in the cooled wood fibre cellulose solution of step 2, get gel; Four, the gel that step 3 is obtained namely gets the lignocellulose aerogel after critical point drying, supercritical drying or lyophilize.
Present embodiment has following beneficial effect:
One, lignocellulose aerogel dissolved efficiency in ionic liquid of preparing of existing method is lower, at least need the above dissolution time of 4h, and lignocellulose aerogel dissolution time in ionic liquid of the preparation method that present embodiment provides is no more than 20min, demand that can satisfying the market;
Two, the preparation method that provides of present embodiment, preparation process is simple, does not need expensive device, extensive, the with low cost and environment-friendly and green of raw material sources, the preparation method is safe, can not bring pollution to environment;
Three, the lignocellulose aerogel of present embodiment method preparation can directly precipitate gelling in non-solvent, does not need freeze thawing treatment repeatedly;
Four, preparation method's process of providing of present embodiment is simple, and technique is easily controlled.
Five, xylon gas's gel of the preparation method preparation that provides of present embodiment is of many uses, can be used for sound insulation, thermal insulation, oil suction, wrapping material, energy storage material, load nano particle, carbon aerogels presoma etc., belong to high value added product, have wide application prospects.
Embodiment two: what present embodiment was different from embodiment one is: the lignocellulosic material described in step 1 is the biomass material that contains xylogen, wherein, the biomass material that contains xylogen comprises Wood waste, papermaking residue, the non-edible part of farm crop or resource crop.Other is identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is: the lignocellulosic material described in step 1 mixes with the ratio that ionic liquid is 0.5～15:100 in mass ratio.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is: the lignocellulosic material described in step 1 mixes with the ratio that ionic liquid is 1～10:100 in mass ratio.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is: the lignocellulosic material described in step 1 mixes for the ratio of 5:100 in mass ratio with ionic liquid.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to five is: the ionic liquid described in step 1 is the alkyl phosphate salt of carboxylate salt, dialkylimidazolium kind phosphate ester salt, N-alkyl pyridine kind phosphate ester salt or quaternary amines of chloro salt, dialkylimidazolium class carboxylate salt, N-alkyl pyridine class carboxylate salt, the quaternary amines of quaternary amines.Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is: 1-allyl group-3-Methylimidazole villaumite ionic liquid, 1-butyl-3-Methylimidazole villaumite ionic liquid, 1-butyl-2,3-methylimidazole villaumite, 1-butyl-3-Methylimidazole acetate, 1-butyl-3-ethyl imidazol(e) dicyan amine salt or 1-alkyl-3-Methylimidazole ionic liquid.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is: being heated to 150～180 ℃ and stirring 5～8min described in step 1.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is: being heated to 170 ℃ and stirring 6min described in step 1.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different from one of embodiment one to nine is: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 150～200 ℃, rotating speed is to stir 5～30min under the condition of 300～600rpm, after perhaps at room temperature stirring 5～30min with the speed of 100～300rpm, speed with 1～10 ℃/min is warming up to 150～200 ℃ again, at rotating speed is to stir under the condition of 300～600rpm.Other is identical with one of embodiment one to nine.
Embodiment 11: what present embodiment was different from one of embodiment one to ten is: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 160～180 ℃, rotating speed is to stir 10～20min under the condition of 400～500rpm, after perhaps at room temperature stirring 10～20min with the speed of 150～250rpm, speed with 4～6 ℃/min is warming up to 160～180 ℃ again, at rotating speed is to stir under the condition of 400～500rpm.Other is identical with one of embodiment one to ten.
Embodiment 12: what present embodiment was different from one of embodiment one to 11 is: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 170 ℃, rotating speed is to stir 15min under the condition of 450rpm, after perhaps at room temperature stirring 15min with the speed of 200rpm, speed with 5 ℃/min is warming up to 170 ℃ again, at rotating speed is to stir under the condition of 450rpm.Other is identical with one of embodiment one to 11.
Embodiment 13: what present embodiment was different from one of embodiment one to 12 is: concrete grammar in step 2, that solution is cooling is: at room temperature placing 2～4h, is perhaps freezing 2～4h under 0～-40 ℃ of condition in temperature.Other is identical with one of embodiment one to 12.
Embodiment 14: what present embodiment was different from one of embodiment one to 13 is: concrete grammar in step 2, that solution is cooling is: at room temperature placing 3h, is perhaps freezing 3h under-10～-30 ℃ of conditions in temperature.Other is identical with one of embodiment one to 13.
Embodiment 15: what present embodiment was different from one of embodiment one to 14 is: the non-solvent described in step 3 is a kind of of deionized water, acetone, dimethyl sulfoxide (DMSO), methyl alcohol, ethanol, the trimethyl carbinol, hexanaphthene or any two kinds of mixed solutions that are mixed by any ratio wherein.Other is identical with one of embodiment one to 14.
Embodiment 16: present embodiment is different from one of embodiment one to 15 is that the drying mode described in step 4 is that lyophilize, drying medium are that critical point drying or the drying medium of carbonic acid gas is the supercritical drying of carbonic acid gas.Other is identical with one of embodiment one to 15.
By following verification experimental verification beneficial effect of the present invention:
Test 1
The method of a kind of quick dissolving mountain jute lignocellulose aerogel of this test, specifically carry out according to following steps:
One, get mountain jute Wood waste, water cleans up, be dried to anhydrous rear pulverizing and cross 60～80 eye mesh screens, then will get the mountain jute wood powder of 5g and the 1-allyl group of 100g-3-Methylimidazole villaumite ionic liquid mixes, at 150 ℃ of temperature, after carrying out magnetic agitation 5min with the rotating speed of 300rpm, get wood powder mountain jute ionic liquid solution; Two, the wood powder mountain jute ionic liquid solution that step 1 is obtained is at room temperature placed 6h; Three, add the 200mL deionized water in the cooling wood powder mountain jute ionic liquid solution of step 2 after, displacement obtains mountain jute lignocellulose gel; Four, the mountain jute lignocellulose gel that step 3 is obtained, the supercritical drying through take carbonic acid gas as drying medium namely obtains mountain jute lignocellulose aerogel.
Fig. 1 is the SEM figure of the mountain jute lignocellulose aerogel of this test preparation, and the mountain yellowwood lignocellulose that can draw dissolving by Fig. 1 is cross-linked with each other and forms typical aerogel structure.
Test 2
The method that a kind of quick dissolving lignocellulose of this test prepares aerogel is with the difference of testing 1: lignocellulosic material used is maize peel.Other step and parameter are identical with test 1.
Fig. 2 is the SEM figure of the maize peel lignocellulose aerogel of preparation, and the maize peel lignocellulose of dissolving has dissolved and formed three-dimensional net structure as seen from Figure 2.
Test 3
The method that a kind of quick dissolving lignocellulose of this test prepares aerogel is with the difference of testing 1: lignocellulosic material used is maize straw.Other step and parameter are identical with test 1.
Fig. 3 is the SEM figure of the maize straw lignocellulose aerogel of preparation, can see that by Fig. 3 the corn structure dissolved, and form vesicular structure.
Test 4
The method that a kind of quick dissolving lignocellulose of this test prepares aerogel is with the difference of testing 1: lignocellulosic material used is China fir.Other step and parameter are identical with test 1.
Fig. 4 is the SEM figure of the wooden cellulose aerogels of China fir of preparation, and the aerogel of can China fir being made after dissolving by Fig. 4 has vesicular structure.
Test 5
The method that a kind of quick dissolving lignocellulose of this test prepares aerogel is with the difference of testing 1: lignocellulosic material used is bamboo.Other step and parameter are identical with test 1.
Fig. 5 can draw by Fig. 5 the three-dimensional net structure that bamboo lignocellulose aerogel has porous for the SEM figure of the bamboo lignocellulose aerogel of preparation.
Claims (10)
1. a quick dissolving lignocellulose prepares the method for aerogel, it is characterized in that utilizing the lignocellulose aerogel to complete according to the following steps: one, to get lignocellulosic material after washing removal of impurities, drying and pulverizing, cross 40～200 eye mesh screens, then after the ratio that is 0.1～20:100 in mass ratio with lignocellulosic material and ionic liquid is mixed, after being heated to 150～200 ℃ of stirring 5～20min, get the wood fibre cellulose solution; Two, mentioned solution is cooling; Three, add non-solvent in the cooled wood fibre cellulose solution of step 2, get gel; Four, the gel that step 3 is obtained namely gets the lignocellulose aerogel after critical point drying, supercritical drying or lyophilize.
2. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the lignocellulosic material described in step 1 is the biomass material that contains xylogen, wherein, the biomass material that contains xylogen comprises Wood waste, papermaking residue, the non-edible part of farm crop or resource crop.
3. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the lignocellulosic material described in step 1 and ionic liquid are that the ratio of 0.5～10:100 is mixed in mass ratio.
4. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the ionic liquid described in step 1 is the alkyl phosphate salt of carboxylate salt, dialkylimidazolium kind phosphate ester salt, N-alkyl pyridine kind phosphate ester salt or quaternary amines of chloro salt, dialkylimidazolium class carboxylate salt, N-alkyl pyridine class carboxylate salt, the quaternary amines of quaternary amines.
5. a kind of quick dissolving lignocellulose according to claim 4 prepares the method for aerogel, it is characterized in that the ionic liquid described in step 1 is 1-allyl group-3-Methylimidazole villaumite ionic liquid, 1-butyl-3-Methylimidazole villaumite ionic liquid, 1-butyl-2,3-methylimidazole villaumite, 1-butyl-3-Methylimidazole acetate, 1-butyl-3-ethyl imidazol(e) dicyan amine salt or 1-alkyl-3-Methylimidazole ionic liquid.
6. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that 150～180 ℃ of stirring 5～8min that are heated to described in step 1.
7. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 150～200 ℃, rotating speed is to stir 5～30min under the condition of 300～600rpm, after perhaps at room temperature stirring 5～30min with the speed of 100～300rpm, then being warming up to 150～200 ℃ with the speed of 1～10 ℃/min, is to stir under the condition of 300～600rpm at rotating speed.
8. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that concrete grammar in step 2, that solution is cooling is: at room temperature placing 2～4h, is perhaps freezing 2～4h under 0～-40 ℃ of condition in temperature.
9. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the non-solvent described in step 3 is a kind of of deionized water, acetone, dimethyl sulfoxide (DMSO), methyl alcohol, ethanol, the trimethyl carbinol, hexanaphthene or any two kinds of mixed solutions that are mixed by any ratio wherein.
10. a kind of quick dissolving lignocellulose according to claim 1 prepares the method for aerogel, it is characterized in that the drying mode described in step 4 is that lyophilize, drying medium are that critical point drying or the drying medium of carbonic acid gas is the supercritical drying of carbonic acid gas.
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