CN103146017B - Method for preparing aerogel by quickly dissolving lignocellulose - Google Patents
Method for preparing aerogel by quickly dissolving lignocellulose Download PDFInfo
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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 of preparing aerogel.
Background technology
Along with the environmental pollution that quick disappearance and the petroleum chemicals consumption of petroleum resources cause, start to make the whole world to start to pay close attention to reproducible Wooden Biomass resource as the alternate resources that can replace petrochemical complex resource.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, again by the tight embedding of xylogen, mutually combines and becomes firm cell walls.Wherein Mierocrystalline cellulose is about 35 – 50%, hemicellulose is 20 – 35%, and xylogen is about 5 – 30%.
But in current " 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 taking phenylpropyl alcohol alkane as unit, connect by ehter bond and C-C the amorphous high polymer forming.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, owing to lacking suitable technology and convert it into the material of high value, most xylogen is used to burn.In the new technology of continual exploitation, should comprise all components in lignocellulose (comprising xylogen) is converted into type material, for example lignocellulose aerogel, to cater to better all challenges of environment, economy, science and technology.With traditional inorganic aerogels (SiO
2, TiO
2and Fe
2o
3) compare, Polymer Gas gel has higher physical strength, can bear higher surging force.Meanwhile, 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 standing in the breach is dissolved in lignocellulose in working medium exactly.Therefore, we have used a class biomacromolecule to be had to 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 the 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 completely.But current dissolving technology needs at least time of 4h, conventionally to lengthen mechanical stirring fast, could completely lignocellulose be dissolved, and preparing in the process of lignocellulose aerogel, also need to make polymer generation physical crosslinking by frozen-thaw process repeatedly, 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.
Quick dissolving lignocellulose is prepared a method for aerogel, specifically carries out according to the following steps:
One, get lignocellulosic material after washing removal of impurities, being dried and pulverizing, cross 40~200 eye mesh screens, then after the ratio that is 0.1~20:100 in mass ratio by lignocellulosic material and ionic liquid is mixed, be heated to 150~200 DEG C and stir after 5~20min, obtain wood fibre cellulose solution; Two, by cooling above-mentioned solution; Three, in the cooled wood fibre cellulose solution of step 2, add non-solvent, obtain gel; Four, gel step 3 being obtained, after critical point drying, supercritical drying or lyophilize, obtains lignocellulose aerogel.
The present invention has following beneficial effect:
One, lignocellulose aerogel dissolved efficiency in ionic liquid that existing method is prepared is lower, at least need dissolution time more than 4h, and lignocellulose aerogel dissolution time in ionic liquid of preparation method provided by the invention is no more than 20min, can meet the demand in 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, preparation method is safe, can not bring pollution to environment;
Three, the lignocellulose aerogel that prepared by the inventive method 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 that prepared by preparation method 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 DEG C.Because used ionic liquid easily decomposes at higher temperature, the temperature of heating can not be higher than 200 DEG C, and the time of heating can not exceed 20min.
Brief description of the drawings
Fig. 1 is the SEM figure of the test 1 mountain jute lignocellulose aerogel making;
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 is prepared the method for aerogel, specifically carry out according to the following steps:
One, get lignocellulosic material after washing removal of impurities, being dried and pulverizing, cross 40~200 eye mesh screens, then after the ratio that is 0.1~20:100 in mass ratio by lignocellulosic material and ionic liquid is mixed, be heated to 150~200 DEG C and stir after 5~20min, obtain wood fibre cellulose solution; Two, by cooling above-mentioned solution; Three, in the cooled wood fibre cellulose solution of step 2, add non-solvent, obtain gel; Four, gel step 3 being obtained, after critical point drying, supercritical drying or lyophilize, obtains lignocellulose aerogel.
Present embodiment has following beneficial effect:
One, lignocellulose aerogel dissolved efficiency in ionic liquid that existing method is prepared is lower, at least need dissolution time more than 4h, and lignocellulose aerogel dissolution time in ionic liquid of the preparation method that present embodiment provides is no more than 20min, can meet the demand in market;
Two, the preparation method that present embodiment provides, preparation process is simple, does not need expensive device, extensive, the with low cost and environment-friendly and green of raw material sources, preparation method is safe, can not bring pollution to environment;
Three, the lignocellulose aerogel that prepared by present embodiment method can directly precipitate gelling in non-solvent, does not need freeze thawing treatment repeatedly;
Four, preparation method's process that present embodiment provides is simple, and technique is easily controlled.
Xylon gas's gel prepared by the preparation method that five, present embodiment provides 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: present embodiment is different from embodiment one: 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: present embodiment is different from embodiment one or two: 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: present embodiment is different from one of embodiment one to three: 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: present embodiment is different from one of embodiment one to four: the lignocellulosic material described in step 1 mixes with the ratio that ionic liquid is 5:100 in mass ratio.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the alkyl phosphate salt of carboxylate salt, dialkylimidazolium kind phosphate ester salt, N-alkyl pyridine kind phosphate ester salt or the quaternary amines of chloro salt that the ionic liquid described in step 1 is quaternary amines, dialkylimidazolium class carboxylate salt, N-alkyl pyridine class carboxylate salt, quaternary amines.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: 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: present embodiment is different from one of embodiment one to seven: described in step 1 be heated to 150~180 DEG C stir 5~8min.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: described in step 1 be heated to 170 DEG C stir 6min.Other is identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 150~200 DEG C, rotating speed is to stir 5~30min under the condition of 300~600rpm, or at room temperature stir after 5~30min with the speed of 100~300rpm, be warming up to 150~200 DEG C with the speed of 1~10 DEG C/min again, under the condition that is 300~600rpm at rotating speed, stir.Other is identical with one of embodiment one to nine.
Embodiment 11: present embodiment is different from one of embodiment one to ten: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 160~180 DEG C, rotating speed is to stir 10~20min under the condition of 400~500rpm, or at room temperature stir after 10~20min with the speed of 150~250rpm, be warming up to 160~180 DEG C with the speed of 4~6 DEG C/min again, under the condition that is 400~500rpm at rotating speed, stir.Other is identical with one of embodiment one to ten.
Embodiment 12: present embodiment is different from one of embodiment one to 11: the stirring described in step 1 is magnetic agitation or mechanical stirring, wherein, the described temperature that is stirred in is 170 DEG C, rotating speed is to stir 15min under the condition of 450rpm, or at room temperature stir after 15min with the speed of 200rpm, be warming up to 170 DEG C with the speed of 5 DEG C/min again, under the condition that is 450rpm at rotating speed, stir.Other is identical with one of embodiment one to 11.
Embodiment 13: present embodiment is different from one of embodiment one to 12: in step 2 by concrete grammar cooling solution be: at room temperature place 2~4h, or be freezing 2~4h under 0~-40 DEG C of condition in temperature.Other is identical with one of embodiment one to 12.
Embodiment 14: present embodiment is different from one of embodiment one to 13: in step 2 by concrete grammar cooling solution be: at room temperature place 3h, or be freezing 3h under-10~-30 DEG C of conditions in temperature.Other is identical with one of embodiment one to 13.
Embodiment 15: present embodiment is different from one of embodiment one to 14: 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: the supercritical drying that the critical point drying that what present embodiment was different from one of embodiment one to 15 the is drying mode described in step 4 is lyophilize, drying medium is carbonic acid gas or drying medium are 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 1-allyl group-3-Methylimidazole villaumite ionic liquid of 100g mixes, at 150 DEG C of temperature, carry out after magnetic agitation 5min with the rotating speed of 300rpm, obtain wood powder mountain jute ionic liquid solution; Two, wood powder mountain jute ionic liquid solution step 1 being obtained is at room temperature placed 6h; Three, in the cooling wood powder mountain jute ionic liquid solution of step 2, add after 200mL deionized water, displacement obtains mountain jute lignocellulose gel; Four, mountain jute lignocellulose gel step 3 being obtained, through the supercritical drying taking carbonic acid gas as drying medium, obtains mountain jute lignocellulose aerogel.
Fig. 1 is the SEM figure of the mountain jute lignocellulose aerogel of this test preparation, can show that the mountain yellowwood lignocellulose of dissolving is cross-linked with each other form typical aerogel structure by Fig. 1.
Test 2
The method that a kind of quick dissolving lignocellulose of this test is prepared aerogel is with the difference of test 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 dissolving as seen from Figure 2 has dissolved and formed three-dimensional net structure.
Test 3
The method that a kind of quick dissolving lignocellulose of this test is prepared aerogel is with the difference of test 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 corn structure dissolves, and form vesicular structure by Fig. 3.
Test 4
The method that a kind of quick dissolving lignocellulose of this test is prepared aerogel is with the difference of test 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 up after dissolving of Fig. 4 has vesicular structure.
Test 5
The method that a kind of quick dissolving lignocellulose of this test is prepared aerogel is with the difference of test 1: lignocellulosic material used is bamboo.Other step and parameter are identical with test 1.
Fig. 5 is the SEM figure of the bamboo lignocellulose aerogel of preparation, can show that by Fig. 5 bamboo lignocellulose aerogel has the three-dimensional net structure of porous.
Claims (5)
1. a quick dissolving lignocellulose is prepared the method for aerogel, it is characterized in that utilizing lignocellulose aerogel to complete according to the following steps: one, to get lignocellulosic material after washing removal of impurities, being dried and pulverizing, cross 40~200 eye mesh screens, then after the ratio that is 0.1~20:100 in mass ratio by lignocellulosic material and ionic liquid is mixed, be heated to 150~200 DEG C and stir after 5~20min, obtain wood fibre cellulose solution; Two, by cooling above-mentioned solution; Three, in the cooled wood fibre cellulose solution of step 2, add non-solvent, obtain gel; Four, gel step 3 being obtained, after critical point drying, supercritical drying or lyophilize, obtains lignocellulose aerogel;
Lignocellulosic material described in step 1 is the biomass material that contains xylogen, and wherein, biomass material comprises Wood waste, papermaking residue, the non-edible part of farm crop or resource crop;
Stirring described in step 1 is magnetic agitation or mechanical stirring, and wherein, the described temperature that is stirred in is 150~200 DEG C, under the condition that rotating speed is 300~600rpm, stirs 5~20min;
Ionic liquid described in step 1 is 1-butyl-2,3-methylimidazole villaumite, 1-butyl-3-Methylimidazole acetate or 1-butyl-3-ethyl imidazol(e) dicyan amine salt;
In step 2, by concrete grammar cooling solution be: at room temperature place 2~4h.
2. a kind of quick dissolving lignocellulose according to claim 1 is prepared 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.
3. a kind of quick dissolving lignocellulose according to claim 1 is prepared the method for aerogel, it is characterized in that 150~180 DEG C of stirring 5~8min that are heated to described in step 1.
4. a kind of quick dissolving lignocellulose according to claim 1 is prepared 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.
5. a kind of quick dissolving lignocellulose according to claim 1 is prepared the method for aerogel, it is characterized in that the drying mode described in step 4 is the supercritical drying that lyophilize, the drying medium critical point drying that is carbonic acid gas or drying medium are carbonic acid gas.
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