CN104861180A - Method for efficiently dissolving full components of plant fiber - Google Patents
Method for efficiently dissolving full components of plant fiber Download PDFInfo
- Publication number
- CN104861180A CN104861180A CN201510268714.5A CN201510268714A CN104861180A CN 104861180 A CN104861180 A CN 104861180A CN 201510268714 A CN201510268714 A CN 201510268714A CN 104861180 A CN104861180 A CN 104861180A
- Authority
- CN
- China
- Prior art keywords
- vegetable fibre
- ionic liquid
- total composition
- plant fiber
- composition high
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004090 dissolution Methods 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002657 fibrous material Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 239000002608 ionic liquid Substances 0.000 claims description 55
- 235000013311 vegetables Nutrition 0.000 claims description 52
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 230000003381 solubilizing effect Effects 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 241000196324 Embryophyta Species 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- -1 filtering separation Substances 0.000 claims description 8
- 239000002023 wood Substances 0.000 claims description 8
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 241000609240 Ambelania acida Species 0.000 claims description 3
- 239000010905 bagasse Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 125000000962 organic group Chemical group 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 125000001424 substituent group Chemical group 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 abstract description 9
- 239000001913 cellulose Substances 0.000 abstract description 7
- 229920005610 lignin Polymers 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 4
- 239000007787 solid Substances 0.000 description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 10
- 239000002904 solvent Substances 0.000 description 9
- 238000013019 agitation Methods 0.000 description 7
- 235000010980 cellulose Nutrition 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 244000166124 Eucalyptus globulus Species 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 2
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- SWJXMGRMNOQWRO-UHFFFAOYSA-N C[n+]1cc[nH]c1.COP([O-])(=O)OC Chemical compound C[n+]1cc[nH]c1.COP([O-])(=O)OC SWJXMGRMNOQWRO-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229920002522 Wood fibre Polymers 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 1
- MEMNKNZDROKJHP-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;methyl sulfate Chemical compound COS([O-])(=O)=O.CCCCN1C=C[N+](C)=C1 MEMNKNZDROKJHP-UHFFFAOYSA-M 0.000 description 1
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- YRGNNOABGRMUKR-UHFFFAOYSA-N Cl(=O)(=O)O.C(CCC)N1CN(C=C1)C Chemical compound Cl(=O)(=O)O.C(CCC)N1CN(C=C1)C YRGNNOABGRMUKR-UHFFFAOYSA-N 0.000 description 1
- KKUKTXOBAWVSHC-UHFFFAOYSA-N Dimethylphosphate Chemical compound COP(O)(=O)OC KKUKTXOBAWVSHC-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 235000019687 Lamb Nutrition 0.000 description 1
- 235000011609 Pinus massoniana Nutrition 0.000 description 1
- 241000018650 Pinus massoniana Species 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 244000305267 Quercus macrolepis Species 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GUBGYTABKSRVRQ-QRZGKKJRSA-N beta-cellobiose Chemical compound OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QRZGKKJRSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011122 softwood Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention belongs to the technical field of processing of plant fiber and discloses a method for efficiently dissolving full components of plant fiber. The method comprises steps as follows: a plant fiber material is added to a water solution of an ion liquid, uniformly stirred and mixed and subjected to a dissolution reaction in a microwave environment at the temperature of 150 DEG C-180 DEG C, the stirring speed ranges from 200 rpm to 280 rpm, and the reaction time ranges from 15 min to 30 min; residues obtained after dissolution are separated centrifugally, and a plant fiber solution is obtained. The proper ion liquid and a dissolution process condition are selected, cellulose and lignin in the plant fiber can be dissolved simultaneously, and the dissolution rate of the plant fiber can be up to 90% or even higher than 95%.
Description
Technical field
The invention belongs to vegetable fibre processing technology field, be specifically related to a kind of method of vegetable fibre total composition high-efficiency dissolution.
Background technology
At occurring in nature, the reserves of xylogen are only second to Mierocrystalline cellulose, and all regenerate with the speed of 5,000,000,000 tons every year.Pulp and paper industry will isolate about 1.4 hundred million tons of Mierocrystalline celluloses every year from plant, obtain the xylogen byproduct of about 5,000 ten thousand tons simultaneously, but up to now, the xylogen more than 95% still directly enters rivers with " black liquor " or burns after concentrating, and is seldom utilized effectively.The development and utilization of lignocellulose is significant to the resource and energy dilemma that solve facing mankind.
The sepn process of current lignocellulose is mainly carried out under acidity or alkaline condition, or adopt small molecules low boiling point organic solvent, as ether, dioxane, benzene, ethanol etc., aforesaid method exists that dissolving step is loaded down with trivial details, dissolution conditions is harsh, acid, the disposable consumption of alkali, organic solvent boiling point is low, use is dangerous large, the problems such as discharging of waste liquid amount is large, environmental pollution is serious, especially isolated lignin structure is seriously damaged, and there is disadvantageous effect to its follow-up deep processing.In addition, complex structure in wood fibre and there is a large amount of hydrogen bonds, causes its total composition dissolution rate not high, and this becomes and hinders one of the biomass resource utilization problem being badly in need of improving.
Ionic liquid at room temperature is the class green material occurred in recent years, has that steam forces down, character controllable, solvability are good, thermostability advantages of higher, has broad application prospects with being separated in lignocellulose in dissolving.Ionic liquid gets most of the attention with its distinctive advantageous property, enjoys the good reputation of " green solvent ", and the application preparing etc. numerous areas at chemosynthesis, biocatalysis, extracting and separating, matrix material is also concerned day by day.
Ionic liquid has good solubility energy to biomass one-component.(the Swatloski RP such as Swatloski; Spear S K; Holbrey J D et al.Dissolution of cellose with ionic liquids [J] .Journal ofthe American Chemical Society, 2002,124 (18)) find that some alkyl substituted imidazole ionic liquid can dissolving cellulos effectively.In studied ionic liquid, 1-butyl-3-Methylimidazole chlorate ([C
4mim] Cl) show that excellent dissolving power---the solubilized 10wt% polymerization degree is the Mierocrystalline cellulose of 1000 at 100 DEG C.(the Ren J L such as Ren; Sun R C; Liu C F et al.Acetylation of wheat strawhemicelluloses in ionic liquid using iodine as a catalyst [J] .Carbohydrate Polymers, 2007,70 (4)) with ionic liquid [C
4mim] Cl be solvent achieve hemicellulose dissolve.For the dissolving of xylogen in ionic liquid, also there are some researches show, ionic liquid 1,3-methylimidazole Methylsulfate ([Mmim] [CH
3sO
4]) and 1-butyl-3-methylimidazolium methylsulfate ([C
4mim] [CH
3sO
4]) at room temperature getting final product dissolved lignin's sample, solubleness is about 74g/L and 62g/L respectively, and when being heated to 50 ~ 70 DEG C, xylogen sample can be dissolved in rapidly wherein, and solubleness can reach 275 ~ 344g/L (Pu Y Q; Jiang N; Ragauskas A J.Ionic liquid as a green solvent for lignin [J] .Journal of WoodChemistry and Technology, 2007,27 (1)).(the Zhou Hongxia such as Zhou Hongxia, Li Lu, Liu Shiwei, Yu Shitao, Liu Fusheng, Xie Congxia. phosphate-based ionic liquid is to the solubility property [J] of xylogen. polymer material science and engineering, 2012, 28 (3)) with five kinds of Phosphate Ionic Liquids, xylogen is dissolved, find ionic liquid 1, 3-methylimidazole dimethyl phosphate salt [Mmim] DMP is best to the solubility property of xylogen, 120min is stirred at 70 DEG C, lignin dissolution Du Keda 45%, but the solubleness of xylogen is still on the low side under this condition, and the dissolving just to xylogen single-component.
And total composition solute effect does not obviously have single component dissolving so obvious.(the Fort D A such as Fort; RemsingR C; Swatloski R P et al.Can ionic liquids dissolve wood? Processing and analysis oflignocellulosic materials with 1-n-butyl-3-methylimidazolium chloride [J] .GreenChemistry, 2007,9 (1)) Primary Study Pinus massoniana Lamb, poplar, Eucalyptus and oak is at [C
4mim] dissolving situation in Cl/ dimethyl sulfoxide (DMSO) (DMSO) solvent system, research finds that not pretreated wood fibre heats 24h and can be partly dissolved at 100 DEG C, is poured into by solution in water or ethanol and can be settled out Mierocrystalline cellulose.(the Kilpelainen I such as Kilpelainen; Xie H; King A et al.Dissolution of wood in ionic liquids [J] .Journalof Agricultural and Food Chemistry, 2007,55 (22)) also find that softwood and hardwood all can be partially dissolved in ionic liquid, and the less wood chip of particle can be dissolved in ionic liquid [C completely after 130 DEG C of process 8h
4mim] Cl and [Amim] Cl.But this solvent system has used organic solvent DMSO, there is environmental issue.
Chinese patent 201110059319.8 discloses the method for a kind of ionic liquid separated fiber element and xylogen from plant fiber material, but this method employs organic solvent DMSO equally, and it can only reach 36% to the dissolution rate of vegetable fibre is the highest.Chinese patent 200910012002.1 discloses a kind of ion liquid solvent and is separated xylogen and cellulosic method in lignocellulose, this method with ionic liquid and water for solvent, but adopt the method for this patent can only dissolved lignin, Mierocrystalline cellulose is separated in early stage in solid form, namely cannot reach the object of high-efficiency dissolution Mierocrystalline cellulose and xylogen simultaneously under this patent condition.
Summary of the invention
In order to solve the shortcoming and defect part of above prior art, the object of the present invention is to provide a kind of method of vegetable fibre total composition high-efficiency dissolution.
The object of the invention is achieved through the following technical solutions:
A method for vegetable fibre total composition high-efficiency dissolution, comprises the following steps:
Plant fiber material is joined in ionic liquid aqueous solution, be uniformly mixed, then under the microwave environment of temperature 150 ~ 180 DEG C, carry out solubilizing reaction, stirring velocity 200 ~ 280rpm, reaction times 15 ~ 30min, centrifugation dissolved residue, obtains vegetable fibre solution.
Described vegetable fibre solution can add volatile precipitation agent ethanol or acetone further, separates out aftergrowth fiber, filtering separation, and ionic liquid aqueous solution removes recycling use after moisture and precipitation agent through distillation.
Described ionic liquid consists of A
tenb
one, wherein, cation A
tenfor glyoxaline compound ion, its chemical structural formula is
Substituent R
1and R
2be respectively alkane or the olefines organic group of carbonatoms 1 ~ 10; Negatively charged ion B
onefor halide-ions, acetate ion or phosphate anion; Ionic liquid is 1,3-methylimidazole dimethyl phosphate ionic liquid ([Mmim] DMP) preferably.
Described ionic liquid aqueous solution refers to that the mass ratio of ionic liquid and water is (2 ~ 20): the solution of 1; The mass ratio of preferred ion liquid and water is the solution of 9:1.
Described plant fiber material refers to the Gramineae fibrous material such as the wood raw material such as wood powder, wood chip or awns bar, bagasse, and the add-on of plant fiber material is 2% ~ 10% of ionic liquid aqueous solution weight.
Described microwave environment refers to that heating power is the microwave environment of 500W.
Described solubilizing reaction preferably reacts 20 ~ 30min at 170 ~ 180 DEG C.
Preparation method of the present invention and the product tool obtained have the following advantages and beneficial effect:
(1) the present invention is by selecting suitable ionic liquid and dissolution process condition, and can dissolve the Mierocrystalline cellulose in vegetable fibre and xylogen, the dissolution rate of vegetable fibre can reach 90% simultaneously, and even more than 95%;
(2) the present invention is using the mixing solutions of ionic liquid and water as solvent, and decrease the use of organic solvent, environmental protection also reduces cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
2.0g Eucalyptus powder is joined in the reaction vessel of 100mL clean dried, add the ionic liquid aqueous solution 50g that different types of massfraction is 90% respectively, be magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 200rpm, and control temperature is at 170 DEG C, after reaction 20min, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculate dissolution rate.
Under different sorts ionic liquid aqueous solution condition, the dissolution rate of vegetable fibre is as shown in table 1:
The dissolution rate of vegetable fibre under table 1 different sorts ionic liquid aqueous solution condition
| Ionic liquid kind | [Mmim]DMP | [Amim]Cl | [Bmim]Cl | [Emim]Ac |
| Vegetable fibre dissolution rate (%) | 92.9 | 58.4 | 47.6 | 32.7 |
[Mmim] DMP:1,3-methylimidazole dimethyl phosphate salt;
[Amim] Cl:1-allyl group-3-Methylimidazole villaumite;
[Bmim] Cl:1-butyl-3-Methylimidazole villaumite;
[Emim] Ac:1-ethyl-3-methylimidazole acetate.
As can be seen from table 1 result, the present embodiment is under different types of ionic liquid aqueous solution condition, and the dissolution rate of vegetable fibre all can reach more than 30%, and when ionic liquid is chosen as 1, during 3-methylimidazole dimethyl phosphate salt, the dissolution rate of vegetable fibre can reach more than 90%.
Embodiment 2
2.0g Eucalyptus powder is joined in the reaction vessel of 100mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 50g of different concns (massfraction) respectively, be magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 200rpm, and control temperature is at 170 DEG C, after reaction 20min, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculate dissolution rate.
Under different concns ionic liquid aqueous solution condition, the dissolution rate of vegetable fibre is as shown in table 2:
The dissolution rate of vegetable fibre under table 2 different concns ionic liquid aqueous solution condition
| Ionic liquid concentration (%) | 100 | 90 | 80 | 70 |
| Vegetable fibre dissolution rate (%) | 67.9 | 92.9 | 78.1 | 54.4 |
When can find out that the concentration of ionic liquid aqueous solution is more than 70% by table 2 result, the dissolution rate of vegetable fibre all can reach more than 50%, and when the concentration of ionic liquid aqueous solution is 90%, the dissolution rate of vegetable fibre can reach more than 90%.
Embodiment 3
2.0g Eucalyptus powder is joined in the reaction vessel of 100mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 50g that concentration (massfraction) is 90%, it is magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 280rpm, control temperature is respectively 170 DEG C, 150 DEG C, 130 DEG C, 110 DEG C and 90 DEG C, after reaction 20min, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculate dissolution rate.
At different solubilizing reaction temperature, the dissolution rate of vegetable fibre is as shown in table 3:
The dissolution rate of vegetable fibre at the different solubilizing reaction temperature of table 3
| Temperature of reaction (DEG C) | 170 | 150 | 130 | 110 | 90 |
| Vegetable fibre dissolution rate (%) | 92.9 | 61.3 | 20.7 | 8.9 | 4.3 |
As can be seen from table 3 result, when solubilizing reaction temperature is higher than 150 DEG C, the dissolution rate of vegetable fibre can reach more than 60%, and solvent temperature higher than 170 DEG C time, the dissolution rate of vegetable fibre can reach more than 90%.
Embodiment 4
2.0g Eucalyptus powder is joined in the reaction vessel of 100mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 50g that concentration (massfraction) is 90%, it is magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 280rpm, control temperature be 170 DEG C react 5min, 10min, 15min, 20min and 25min respectively after, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculate dissolution rate.
Under the different solubilizing reaction time, the dissolution rate of vegetable fibre is as shown in table 4:
The dissolution rate of vegetable fibre under the table 4 different solubilizing reaction time
| Reaction times (min) | 25 | 20 | 15 | 10 | 5 |
| Vegetable fibre dissolution rate (%) | 93.4 | 92.9 | 47.6 | 16.8 | 10.2 |
As can be seen from table 4 result, when the solubilizing reaction time is more than 15min, the dissolution rate of vegetable fibre can reach more than 40%, and dissolution time more than 20min time, the dissolution rate of vegetable fibre can reach more than 90%.
Embodiment 5
2.0g Eucalyptus powder is joined in the reaction vessel of 100mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 50g that concentration (massfraction) is 90%, be magnetic agitation in the microwave instrument of 500W respectively at power, stirring velocity is 280rpm, control temperature is 170 DEG C of reaction 20min and reacts 30h under oil bath environment, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculate dissolution rate.
Under microwave environment and oil bath environment, the dissolution rate of vegetable fibre is as shown in table 5:
The dissolution rate of vegetable fibre under the different solubilizing reaction environment of table 5
| Reaction environment | 500W microwave reaction 20min | Oil bath reaction 30h |
| Vegetable fibre dissolution rate (%) | 92.9 | 76.8 |
As can be seen from table 5 result, during 500W microwave reaction 20min, the dissolution rate of vegetable fibre can reach more than 90%, and its effect is better than the effect of reacting 30h under oil bath condition.
Embodiment 6
2.0g awns bar powder is joined in the reaction vessel of 200mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 100g that massfraction is 90%, be magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 250rpm, and control temperature is at 180 DEG C, after reaction 20min, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculating dissolution rate is 96.7%.
Embodiment 7
2.0g bagasse powder is joined in the reaction vessel of 50mL clean dried, add [Mmim] DMP ionic liquid aqueous solution 20g that massfraction is 90%, be magnetic agitation in the microwave instrument of 500W at power, stirring velocity is 250rpm, and control temperature is at 170 DEG C, after reaction 30min, be down to room temperature, centrifugation, obtain vegetable fibre solution and undissolved solid matter, obtain dissolved residue after solid matter cleaning post-drying, calculating dissolution rate is 97.9%.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a method for vegetable fibre total composition high-efficiency dissolution, is characterized in that comprising the following steps:
Plant fiber material is joined in ionic liquid aqueous solution, be uniformly mixed, then under the microwave environment of temperature 150 ~ 180 DEG C, carry out solubilizing reaction, stirring velocity 200 ~ 280rpm, reaction times 15 ~ 30min, centrifugation dissolved residue, obtains vegetable fibre solution.
2. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1, it is characterized in that: described vegetable fibre solution adds volatile precipitation agent ethanol or acetone further, separate out aftergrowth fiber, filtering separation, filtrate removes recycling use after moisture and precipitation agent through distillation.
3. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1 and 2, is characterized in that: described plant fiber material refers to wood powder, wood chip, awns bar or bagasse; The add-on of plant fiber material is 2% ~ 10% of ionic liquid aqueous solution weight.
4. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1 and 2, is characterized in that: described ionic liquid consists of A
tenb
one, wherein, cation A
tenfor glyoxaline compound ion, its chemical structural formula is
Substituent R
1and R
2be respectively alkane or the olefines organic group of carbonatoms 1 ~ 10; Negatively charged ion B
onefor halide-ions, acetate ion or phosphate anion.
5. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 4, is characterized in that: described ionic liquid refers to 1,3-methylimidazole dimethyl phosphate salt.
6. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1 and 2, is characterized in that: described ionic liquid aqueous solution refers to that the mass ratio of ionic liquid and water is (2 ~ 20): the solution of 1.
7. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 6, is characterized in that: described ionic liquid aqueous solution refers to that the mass ratio of ionic liquid and water is the solution of 9:1.
8. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1 and 2, is characterized in that: described microwave environment refers to that heating power is the microwave environment of 500W.
9. the method for a kind of vegetable fibre total composition high-efficiency dissolution according to claim 1 and 2, is characterized in that: described solubilizing reaction refers to reaction 20 ~ 30min at 170 ~ 180 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510268714.5A CN104861180B (en) | 2015-05-22 | 2015-05-22 | A kind of method of string full constituent high-efficiency dissolution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510268714.5A CN104861180B (en) | 2015-05-22 | 2015-05-22 | A kind of method of string full constituent high-efficiency dissolution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104861180A true CN104861180A (en) | 2015-08-26 |
| CN104861180B CN104861180B (en) | 2017-10-20 |
Family
ID=53907394
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510268714.5A Expired - Fee Related CN104861180B (en) | 2015-05-22 | 2015-05-22 | A kind of method of string full constituent high-efficiency dissolution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104861180B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105401303A (en) * | 2015-12-01 | 2016-03-16 | 惠安华晨贸易有限公司 | Environmental friendly cloth preparation method |
| CN106220870A (en) * | 2016-08-09 | 2016-12-14 | 东华大学 | A kind of solvent dissolving plant and method |
| CN106750360A (en) * | 2016-11-22 | 2017-05-31 | 华南理工大学 | A kind of method of the reverse solution system separating lignin of utilization alkali ionic liquid |
| CN108940218A (en) * | 2018-06-30 | 2018-12-07 | 华南理工大学 | A kind of preparation method of heavy metal absorbent-lignin microballoon |
| CN110514609A (en) * | 2019-09-26 | 2019-11-29 | 武汉海关技术中心 | The analyzing detecting method of lead metal element in solid food sample |
| CN110530811A (en) * | 2019-09-26 | 2019-12-03 | 武汉海关技术中心 | The analyzing detecting method of Cd metallic element in solid food sample |
| CN110567775A (en) * | 2019-09-26 | 2019-12-13 | 武汉海关技术中心 | Solid food sample pretreatment method based on ionic liquid |
| CN110609004A (en) * | 2019-09-26 | 2019-12-24 | 武汉海关技术中心 | Analysis and detection method for chromium metal element in solid food sample |
| CN112029119A (en) * | 2020-08-03 | 2020-12-04 | 福建农林大学 | Method for efficiently and quickly dissolving cellulose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807515A (en) * | 2005-01-20 | 2006-07-26 | 中国科学院过程工程研究所 | Method for preparing degradable material using stalk |
| CN101580522A (en) * | 2009-06-11 | 2009-11-18 | 大连工业大学 | Method for separating lignin and cellulose from lignocellulose by using ionic liquid solvent |
| CN101712698A (en) * | 2009-11-25 | 2010-05-26 | 大连工业大学 | Ionic liquid based method for extracting lignin by two-liquid-phase system |
| CN102677510A (en) * | 2011-03-11 | 2012-09-19 | 中国科学院过程工程研究所 | Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid |
-
2015
- 2015-05-22 CN CN201510268714.5A patent/CN104861180B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807515A (en) * | 2005-01-20 | 2006-07-26 | 中国科学院过程工程研究所 | Method for preparing degradable material using stalk |
| CN101580522A (en) * | 2009-06-11 | 2009-11-18 | 大连工业大学 | Method for separating lignin and cellulose from lignocellulose by using ionic liquid solvent |
| CN101712698A (en) * | 2009-11-25 | 2010-05-26 | 大连工业大学 | Ionic liquid based method for extracting lignin by two-liquid-phase system |
| CN102677510A (en) * | 2011-03-11 | 2012-09-19 | 中国科学院过程工程研究所 | Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105401303A (en) * | 2015-12-01 | 2016-03-16 | 惠安华晨贸易有限公司 | Environmental friendly cloth preparation method |
| CN106220870A (en) * | 2016-08-09 | 2016-12-14 | 东华大学 | A kind of solvent dissolving plant and method |
| CN106750360A (en) * | 2016-11-22 | 2017-05-31 | 华南理工大学 | A kind of method of the reverse solution system separating lignin of utilization alkali ionic liquid |
| CN108940218A (en) * | 2018-06-30 | 2018-12-07 | 华南理工大学 | A kind of preparation method of heavy metal absorbent-lignin microballoon |
| CN108940218B (en) * | 2018-06-30 | 2021-01-19 | 华南理工大学 | Preparation method of heavy metal adsorbent-lignin microspheres |
| CN110514609A (en) * | 2019-09-26 | 2019-11-29 | 武汉海关技术中心 | The analyzing detecting method of lead metal element in solid food sample |
| CN110530811A (en) * | 2019-09-26 | 2019-12-03 | 武汉海关技术中心 | The analyzing detecting method of Cd metallic element in solid food sample |
| CN110567775A (en) * | 2019-09-26 | 2019-12-13 | 武汉海关技术中心 | Solid food sample pretreatment method based on ionic liquid |
| CN110609004A (en) * | 2019-09-26 | 2019-12-24 | 武汉海关技术中心 | Analysis and detection method for chromium metal element in solid food sample |
| CN110514609B (en) * | 2019-09-26 | 2022-08-02 | 武汉海关技术中心 | Analysis and detection method for lead metal element in solid food sample |
| CN110567775B (en) * | 2019-09-26 | 2022-08-12 | 武汉海关技术中心 | Solid food sample pretreatment method based on ionic liquid |
| CN112029119A (en) * | 2020-08-03 | 2020-12-04 | 福建农林大学 | Method for efficiently and quickly dissolving cellulose |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104861180B (en) | 2017-10-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104861180A (en) | Method for efficiently dissolving full components of plant fiber | |
| Wen et al. | Production of xylooligosaccharides and monosaccharides from poplar by a two-step acetic acid and peroxide/acetic acid pretreatment | |
| Luo et al. | Promoting enzymatic hydrolysis of lignocellulosic biomass by inexpensive soy protein | |
| Nagarajan et al. | Cellulose II as bioethanol feedstock and its advantages over native cellulose | |
| Rocha et al. | Mass balance of pilot-scale pretreatment of sugarcane bagasse by steam explosion followed by alkaline delignification | |
| Froschauer et al. | Separation of hemicellulose and cellulose from wood pulp by means of ionic liquid/cosolvent systems | |
| Wang et al. | Cellulose extraction from wood chip in an ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl) | |
| Tian et al. | Liquid hot water extraction followed by mechanical extrusion as a chemical-free pretreatment approach for cellulosic ethanol production from rigid hardwood | |
| Zhong et al. | Rapid and efficient microwave-assisted guanidine hydrochloride deep eutectic solvent pretreatment for biological conversion of castor stalk | |
| Jiang et al. | Isolation of cellulose with ionic liquid from steam exploded rice straw | |
| CN103254452B (en) | Preparation method of lignin nanoparticle | |
| Chu et al. | Improving enzymatic saccharification and ethanol production from hardwood by deacetylation and steam pretreatment: insight into mitigating lignin inhibition | |
| Yan et al. | Fractionation of lignin from eucalyptus bark using amine-sulfonate functionalized ionic liquids | |
| Chandra et al. | Enhancing hemicellulose recovery and the enzymatic hydrolysis of cellulose by adding lignosulfonates during the two-stage steam pretreatment of poplar | |
| CN105884907B (en) | A kind of method that straw component separation prepares ultra low viscosity carboxymethyl cellulose | |
| CN111808216B (en) | Method for extracting hemicellulose from biomass by using eutectic solvent | |
| Zhang et al. | Enhancement of enzymatic hydrolysis of lignocellulose by Tetrabutylammonium Hydroxide (TBAOH) and Tetramethylammonium Hydroxide (TMAOH) aqueous solution pretreatment | |
| CN110551295A (en) | Method for separating chemical components of gramineous plants and purifying lignin | |
| CN105418943A (en) | Dissolution method of lignocellulose | |
| Wang et al. | The application of ionic liquids in dissolution and separation of lignocellulose | |
| Cybulska et al. | Lignocellulosic thermochemical pretreatment processes | |
| Long et al. | Ionic liquids: Efficient solvent and medium for the transformation of renewable lignocellulose | |
| Marks et al. | Solvents and ions for pretreatment in lignocellulosic biorefineries | |
| Wang et al. | Efficient preparation of high-purity cellulose from moso bamboo by p-toluenesulfonic acid pretreatment | |
| Hartati et al. | Microwave-assisted urea-based-hydrotropic pretreatment of rice straw: Experimental data and mechanistic kinetic models |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171020 |