CN105908550B - A kind of method of the separation and Extraction lignin from Eucalyptus - Google Patents

A kind of method of the separation and Extraction lignin from Eucalyptus Download PDF

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CN105908550B
CN105908550B CN201610408294.0A CN201610408294A CN105908550B CN 105908550 B CN105908550 B CN 105908550B CN 201610408294 A CN201610408294 A CN 201610408294A CN 105908550 B CN105908550 B CN 105908550B
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eucalyptus
lignin
separation
congruent melting
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CN105908550A (en
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常杰
刘钧
王菊
付严
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South China University of Technology SCUT
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G1/00—Lignin; Lignin derivatives

Abstract

The invention discloses a kind of method of the separation and Extraction lignin from Eucalyptus, comprise the following steps：1) Eucalyptus powder and depth congruent melting solvent are added in reactor, 60 100 DEG C of controlling reaction temperature, stirring reaction 4 10 hours；The depth congruent melting solvent is by lactic acid and benzyltriethylammoinium chloride in molar ratio 1:3‑1:9 is well mixed obtained；2) reaction product is taken out, decompression filters, and washs residue with ethanol, and carrying out rotary evaporation to suction filtration gained filtrate obtains concentrate, and reclaims ethanol；Deionized water is added in concentrate, standing separation obtains the mixed liquor containing sediment；3) above-mentioned mixed liquor is centrifuged, then separation of solid and liquid, gained solid phase is washed with deionized, and cleans namely regenerated lignin.The present invention can effectively extract the lignin in Eucalyptus, and the purity of product is more than 90%.This method technique is simple, mild condition improves biomass resource utilization efficiency, reduces cost.

Description

A kind of method of the separation and Extraction lignin from Eucalyptus
Technical field
The present invention relates to biomass pretreatment and component isolation technics, especially one kind separation and Extraction high-purity from Eucalyptus The method of lignin.
Background technology
Due to having the advantages that yield is big, pollution is low, renewable, biomass is considered as a kind of preferably alternative energy Source.Lignin is that content is only second to one of biomass resource of cellulose in nature, is unique reproducible to contain aromatic structure Material.Lignin is the natural aromatic macromolecule being made up of oxide unit, can be widely applied to synthetic resin, surface-active The fields such as agent, ore dressing flotation agent, refractory material.The separation of lignin and high-valued technology have gradually obtained extensive concern.
Lignocellulosic structure is complicated, intramolecular and intermolecular hydrogen bond be present in cellulose molecular chain, and with multilayer Space structure forms the network structure of high crystalline, while lignin passes through forulic acid or p-Coumaric Acid and hemicellulose side chain Arabinose O-5 positions connect to form the special bridge-type cross-linked structure of lignin-forulic acid-hemicellulose, and lignin and fiber With Van der Waals force or Hydrogenbond between element.Therefore, separating lignin needs to realize high selection of the pretreatment to lignin simultaneously Property effect and the chemical bond to being connected between three kinds of components effectively interrupt.
The traditional main acid system of lignin extraction method, alkaline process and organic solvent method.Wherein, acidity extraction is usually to utilize 72% dense sulfuric acid treatment plant material, dissolves glycan, and is supplemented and hydrolyzed with diluted acid, and the residue remained is sourwood matter Element.The substantial amounts of concentrated sulfuric acid can cause certain economic loss to the seriously corroded of equipment in acid system.Alkalinity extraction is mainly with alkali soluble Liquid causes lignin dissolution under certain condition, and acid is then added into aqueous slkali makes lignin deposit, gained lignin it is more with Lignin salt's form is present, and lignin purity is not high, is unfavorable for lignin deep processing utilization, while easily causes environment dirt Dye.Organic solvent method utilizes organic solvent good dissolubility and effumability, reaches the separation purpose of lignin.The method can Reach ringing so that organic solvent is recovered by distillation.But the shortcomings of inflammable, the volatile and toxicity of organic solvent is high, is present Potential safety hazard.
The content of the invention
It is an object of the invention to provide a kind of system preprocessing biomass based on depth congruent melting solvent selectively to divide From the method for lignin in extraction Eucalyptus, technique needed for this method is simple, processing is rapid, mild condition, and will not cause to add Environmental hazard, the high-efficiency pretreatment of Eucalyptus timber is realized, improve the efficiency of biomass resource utilization, for subsequently high-valued Using providing certain facility.
The object of the invention is achieved through the following technical solutions：
A kind of method of the separation and Extraction lignin from Eucalyptus, comprises the following steps：
1) Eucalyptus powder and depth congruent melting solvent are added in reactor, the mass ratio of Eucalyptus powder and depth congruent melting solvent For 1:10-1:30,60-100 DEG C of controlling reaction temperature, stirring, react 4-10 hours；The depth congruent melting solvent is by lactic acid and benzyl TEBA in molar ratio 1:3-1:9 are well mixed and obtain；
2) reaction product is taken out, decompression filters, and washs residue with ethanol, and carrying out rotary evaporation to suction filtration gained filtrate obtains To concentrate, and reclaim ethanol；Deionized water is added in concentrate, standing separation obtains the mixed liquor containing sediment；
3) above-mentioned mixed liquor is centrifuged, then separation of solid and liquid, gained solid phase is washed with deionized, and cleans as again Raw lignin.
Gained liquid product reclaims depth congruent melting solvent through being evaporated under reduced pressure after the step 3) separation of solid and liquid.
The vacuum distillation is to be carried out using Rotary Evaporators under 50-100 DEG C of water bath condition.
The preparation of the depth congruent melting solvent：At 30-80 DEG C in constant temperature after lactic acid is mixed with benzyltriethylammoinium chloride Shaking table handles 1-4 hours, forms the solution of homogeneous transparent.
Benzyltriethylammoinium chloride and lactic acid mol ratio are 1 in the depth congruent melting solvent:7-1:9.
The Eucalyptus powder is to filter out 20-60 mesh powders after Eucalyptus trunk is crushed.
The volume ratio of the step 2) concentrate and deionized water is 1:5-1:15.
The rotating speed of the step 3) centrifugation is 3000-10000rpm, time 5-25min.
Solid phase obtained by step 3) is cleaned produces recycled wood quality after 60-105 DEG C of drying.
Preferably, 80-90 DEG C of step 1) reaction temperature, 5-8 hours are reacted.
The rotating speed of step 1) stirring is 100-150rpm.
Compared with prior art, the advantages of the present invention are as follows：
1) depth congruent melting solvent (Deep Eutectic Solvent, DES) is employed to pre-process Eucalyptus, in system DES and ethanol can be reused by rotary evaporation to reclaim, and reduce reagent cost to a certain extent, while also effectively drop The low pollution to environment, method have good economy and the feature of environmental protection.
2) present invention uses the lactic acid (LA) that can be recycled and the DES that benzyltriethylammoinium chloride (TEBA) is prepared into molten Agent system pre-processes to Eucalyptus powder, by the regulation to LA in dicyandiamide solution and TEBA mol ratios, makes system optionally The separative efficiency for dissolving the product wooden, whole processing technology each stage obtains is high good with structural intergrity.The present invention can have Effect extracts the lignin in Eucalyptus, it might even be possible to reaches 90-95%, the purity of product is more than 90%.
3) technique needed for this method is simple, handles rapid, mild condition and will not cause additional environmental hazard, realizes High-efficiency pretreatment and component separation to Eucalyptus class plant, improve biomass resource utilization efficiency, reduce cost, solve The low problem of lignin component producing level during Eucalyptus utilizes.
Brief description of the drawings
Fig. 1 is the infrared spectrum of lignin product prepared by the embodiment of the present invention 3.
Fig. 2 is lignin product prepared by the embodiment of the present invention 31C-NMR proton nmr spectras.
Embodiment
By embodiment, the invention will be further described, for especially not dated technological parameter, can refer to conventional skill Art is carried out.
Embodiment 1
1. a kind of method of the Selective Separation lignin from Eucalyptus, is comprised the following steps that：
1) will Eucalyptus trunk crush after filter out 40-60 mesh powders, in vacuum drying chamber in 100 ± 5 DEG C, Dried under the conditions of 0.01Mpa；
2) it is DES (TEBA and LA mol ratios 1 that 1g Eucalyptus powder and 10g are successively added into reactor:9) it is, appropriate to shake Make solid-liquid two-phase mixtures uniform；
3) start reactor, 90 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 8h；
4) question response thing takes out reaction product after being cooled to room temperature after having reacted, and decompression suction filtration is carried out using Buchner funnel, And residue is washed with ethanol, carrying out rotary evaporation in 70 ± 5 DEG C, 0.02Mpa to the filtrate that suction filtration obtains obtains concentrate, and returns Receive ethanol；
5) 50ml deionized waters are added in gained 10g ± 1g concentrates, stands 10 hours, obtain the mixing containing sediment Liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by DES pretreatment with follow-up extraction, and the yield of gained lignin is 77% ± 4%, purity is 95 ± 1%, and the lignin yield is the matter of the lignin quality and lignin in Eucalyptus powder that regenerate Measure ratio.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 93% ± 1%. The ethanol for being used to wash residue in experiment is evaporated under reduced pressure back by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Receive, the rate of recovery is 99% ± 1%.
Embodiment 2
1. a kind of method of the Selective Separation lignin from Eucalyptus, is comprised the following steps that：
1) will Eucalyptus trunk crush after filter out 40-60 mesh powders, in vacuum drying chamber in 100 ± 5 DEG C, Dried under the conditions of 0.01Mpa；
2) it is DES (TEBA and LA mol ratios 1 that 1g Eucalyptus powder and 30g are successively added into reactor:3) it is, appropriate to shake Make solid-liquid two-phase mixtures uniform；
3) start reactor, 90 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 8h；
4) question response thing takes out reaction product after being cooled to room temperature after having reacted, and decompression suction filtration is carried out using Buchner funnel, And residue is washed with ethanol, carrying out rotary evaporation in 70 ± 5 DEG C, 0.02Mpa to the filtrate that suction filtration obtains obtains concentrate, and returns Receive ethanol；
5) 150ml deionized waters are added in gained 30g ± 1g concentrates, stands 10 hours, obtained mixed containing sediment Close liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by DES pretreatment with follow-up extraction, and the yield of gained lignin is 68% ± 4%, purity is 91 ± 1%, and the lignin yield is the matter of the lignin quality and lignin in Eucalyptus powder that regenerate Measure ratio.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 96% ± 1%. The ethanol for being used to wash residue in experiment is evaporated under reduced pressure back by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Receive, the rate of recovery is 98% ± 2%.
Embodiment 3
1. a kind of method of the Selective Separation lignin from Eucalyptus, is comprised the following steps that：
1) will Eucalyptus trunk crush after filter out 40-60 mesh powders, in vacuum drying chamber in 100 ± 5 DEG C, Dried under the conditions of 0.01Mpa；
2) it is DES (TEBA and LA mol ratios 1 that 1g Eucalyptus powder and 30g are successively added into reactor:9) it is, appropriate to shake Make solid-liquid two-phase mixtures uniform；
3) start reactor, 90 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 8 hours；4) after having reacted Question response thing takes out reaction product after being cooled to room temperature, and decompression suction filtration is carried out using Buchner funnel, and washs residue with ethanol, right Obtained filtrate is filtered to obtain concentrate in 70 ± 5 DEG C, 0.02Mpa progress rotary evaporations, and reclaim ethanol；
5) 150ml deionized waters are added in gained 30g ± 1g concentrates, stands 10 hours, obtained mixed containing sediment Close liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by DES pretreatment with follow-up extraction, and the yield of gained lignin is 91% ± 4%, purity is 94 ± 1%, and the lignin yield is the matter of the lignin quality and lignin in Eucalyptus powder that regenerate Measure ratio.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 90% ± 1%. The ethanol for being used to wash residue in experiment is evaporated under reduced pressure back by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Receive, the rate of recovery is 97% ± 2%.
Embodiment 4
1. a kind of method of the selective extraction separating lignin from Eucalyptus, step are as follows：
1) 40-60 mesh powders are filtered out after Eucalyptus trunk is crushed, in 80 ± 5 DEG C, 0.01Mpa in vacuum drying chamber Under the conditions of dry；
2) 1g Eucalyptus powder and 30g DES (TEBA and LA mol ratios 1 are successively added into reactor:7), appropriate shake makes Solid-liquid two-phase mixtures are uniform；
3) start reactor, 90 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 8h；
4) question response thing takes out reaction product after being cooled to room temperature after having reacted, and decompression suction filtration is carried out using Buchner funnel, And residue is washed with ethanol, carrying out rotary evaporation in 70 ± 5 DEG C, 0.02Mpa to the filtrate that suction filtration obtains obtains concentrate, and returns Receive ethanol；
5) 150ml deionized waters are added in gained 30g ± 1g concentrates, stands 10h, obtain the mixing containing sediment Liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by the pretreatment of DES dicyandiamide solutions with follow-up extraction, gained lignin Yield be 89% ± 4%, purity be 92 ± 1%.Lignin quality of the lignin yield for regeneration and wood in Eucalyptus powder The mass values of quality.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 91% ± 1%.It is used to wash the right ethanol of residue in experiment by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Recovery is evaporated under reduced pressure, the rate of recovery is 96% ± 1%.
Embodiment 5
1. a kind of method of the selective extraction separating lignin from Eucalyptus, step are as follows：
1) 40-60 mesh powders are filtered out after Eucalyptus trunk is crushed, in 80 ± 5 DEG C, 0.01Mpa in vacuum drying chamber Under the conditions of dry；
2) 1g Eucalyptus powder and 30g DES (TEBA and LA mol ratios 1 are successively added into reactor:9), appropriate shake makes Solid-liquid two-phase mixtures are uniform；
3) start reactor, 80 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 8h；
4) question response thing takes out reaction product after being cooled to room temperature after having reacted, and decompression suction filtration is carried out using Buchner funnel, And residue is washed with ethanol, carrying out rotary evaporation in 70 ± 5 DEG C, 0.02Mpa to the filtrate that suction filtration obtains obtains concentrate, and returns Receive ethanol；
5) 150ml deionized waters are added in gained 30g ± 1g concentrates, stands 10h, obtain the mixing containing sediment Liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by the pretreatment of DES dicyandiamide solutions with follow-up extraction, gained lignin Yield be 80% ± 3%, purity be 95 ± 1%.Lignin quality of the lignin yield for regeneration and wood in Eucalyptus powder The mass values of quality.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 96% ± 2%.It is used to wash the right ethanol of residue in experiment by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Recovery is evaporated under reduced pressure, the rate of recovery is 98% ± 1%.
Embodiment 6
1. a kind of method of the selective extraction separating lignin from Eucalyptus, step are as follows：
1) 40-60 mesh powders are filtered out after Eucalyptus trunk is crushed, in 80 ± 5 DEG C, 0.01Mpa in vacuum drying chamber Under the conditions of dry；
2) 1g Eucalyptus powder and 30g DES (TEBA and LA mol ratios 1 are successively added into reactor:9), appropriate shake makes Solid-liquid two-phase mixtures are uniform；
3) start reactor, 90 DEG C, fixed rotating speed 100rpm of controlling reaction temperature, react 4h；
4) question response thing takes out reaction product after being cooled to room temperature after having reacted, and decompression suction filtration is carried out using Buchner funnel, And residue is washed with ethanol, carrying out rotary evaporation in 70 ± 5 DEG C, 0.02Mpa to the filtrate that suction filtration obtains obtains concentrate, and returns Receive ethanol；
5) 150ml deionized waters are added in gained 30g ± 1g concentrates, stands 10h, obtain the mixing containing sediment Liquid；
6) 15min is centrifuged with 4000rpm/min rotating speeds to above-mentioned mixed liquor, then be filtered under diminished pressure point with Buchner funnel From；
7) gained solid phase after separation of solid and liquid is washed with deionized, cleans and obtains target product after 80 ± 5 DEG C of drying, i.e., For recycled wood quality.
8) the gained rotated evaporimeter of liquid product is evaporated under reduced pressure under 80 DEG C, 0.02Mpa water bath conditions after separation of solid and liquid Concentrate is obtained, the DES as reclaimed, repetitive cycling uses.
Testing result shows：Eucalyptus powder separates by the pretreatment of DES dicyandiamide solutions with follow-up extraction, gained lignin Yield be 71% ± 4%, purity be 96 ± 1%.Lignin quality of the lignin yield for regeneration and wood in Eucalyptus powder The mass values of quality.The rotated evaporimeters of DES are evaporated under reduced pressure recovery under 80 DEG C, 0.02Mpa water bath conditions, and the rate of recovery is 95% ± 1%.It is used to wash the right ethanol of residue in experiment by Rotary Evaporators under 70 ± 5 DEG C, 0.02Mpa water bath conditions Recovery is evaporated under reduced pressure, the rate of recovery is 97% ± 2%.
3441cm in Fig. 1-1The strong absworption peak at place represents lignin hydroxyl O-H stretching vibrations；2900cm-1The absworption peak at place Represent C-H stretching vibrations in methyl, methylene；1710cm-1Place's absworption peak is C=O stretching vibrations, 1600cm-1,1505cm-1Place Absworption peak is lignin phenyl ring skeletal vibration；1230cm-1It is that C-C adds C-O stretching vibrations to locate absworption peak；1150cm-1Locate absworption peak Belong to the anti-stretching vibrations of C-O-C in lignin.Absworption peak 1505cm-1<1470cm-1, show that lilac base content is higher, 830cm-1It is typical broadleaf lignin characteristic peak that place, which only has an absworption peak,.The infrared spectrum of lignin product and the mill of Eucalyptus The infrared spectrum of wooden lignin sample is similar, and this shows that DES used in this research is separating to lignin efficient selective The stabilization of gained lignin product structure is ensure that simultaneously.
In Fig. 2, shift value 150,103ppm is lilac base (S) signal.145ppm is guaiacyl (G) cell signal. 131ppm is non-etherificate S/G units, and 117ppm small-signal peak represents p-hydroxyphenyl unit (H), and this shows separating obtained wooden Element is by lilac base, guaiacyl and a small amount of p-hydroxyphenyl construction unit composition.65ppm shows the presence of β-O-4 units, Qiang Feng representatives-OCH at 54ppm3.Nuclear magnetic spectrogram result is similar to Eucalyptus Milled wood lignin, further illustrates in separation process Lignin structure is not by larger destruction.

Claims (10)

  1. A kind of 1. method of the separation and Extraction lignin from Eucalyptus, it is characterised in that comprise the following steps：
    1) Eucalyptus powder and depth congruent melting solvent are added in reactor, the mass ratio of Eucalyptus powder and depth congruent melting solvent is 1: 10-1:30,60-100 DEG C of controlling reaction temperature, stirring, react 4-10 hours；The depth congruent melting solvent is by benzyl triethyl ammonium chlorine Change ammonium and lactic acid in molar ratio 1:3-1:9 is well mixed obtained；
    2) taking-up reaction product, decompression filters, and washs residue with ethanol, suction filtration gained filtrate progress rotary evaporation is obtained dense Contracting liquid, and reclaim ethanol；Deionized water is added in concentrate, standing separation obtains the mixed liquor containing sediment；
    3) above-mentioned mixed liquor is centrifuged, then separation of solid and liquid, gained solid phase is washed with deionized, and cleans namely regenerated wood Quality.
  2. 2. according to the method for claim 1, it is characterised in that gained liquid product is through subtracting after the step 3) separation of solid and liquid Pressure is distilled to recover depth congruent melting solvent.
  3. 3. according to the method for claim 2, it is characterised in that the vacuum distillation is in 50-100 using Rotary Evaporators Carried out under DEG C water bath condition.
  4. 4. according to the method described in claim 1 or 2 or 3, it is characterised in that the preparation of the depth congruent melting solvent：By lactic acid 1-4 hours are handled in constant-temperature table at 30-80 DEG C after being mixed with benzyltriethylammoinium chloride, form the solution of homogeneous transparent.
  5. 5. according to the method for claim 4, it is characterised in that in the depth congruent melting solvent benzyltriethylammoinium chloride with Lactic acid mol ratio is 1:7-1:9.
  6. 6. according to the method described in claim 1 or 2 or 3, it is characterised in that the Eucalyptus powder is after Eucalyptus trunk is crushed Filter out 20-60 mesh powders.
  7. 7. according to the method described in claim 1 or 2 or 3, it is characterised in that the step 2) concentrate and the body of deionized water Product is than being 1:5-1:15.
  8. 8. according to the method described in claim 1 or 2 or 3, it is characterised in that the rotating speed of the step 3) centrifugation is 3000- 10000rpm, time 5-25min；Gained solid phase is cleaned produces recycled wood quality after 60-105 DEG C of drying.
  9. 9. according to the method described in claim 1 or 2 or 3, it is characterised in that 80-90 DEG C of step 1) reaction temperature, react 5-8 Hour.
  10. 10. according to the method described in claim 1 or 2 or 3, it is characterised in that the rotating speed of step 1) stirring is 100-150rpm.
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