CN109778582A - The method of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass - Google Patents
The method of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass Download PDFInfo
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- CN109778582A CN109778582A CN201711114052.1A CN201711114052A CN109778582A CN 109778582 A CN109778582 A CN 109778582A CN 201711114052 A CN201711114052 A CN 201711114052A CN 109778582 A CN109778582 A CN 109778582A
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Abstract
The invention discloses a kind of methods of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass.In a kettle, biomass material, recyclable solvent tetrahydrofurfuryl alcohol and a certain amount of water is added, under certain conditions, it is reacted, it is separated by filtration, obtained solid is cellulose products, and solvent portions pass through aqueous precipitation, isolated solid is lignin product, and hemicellulose dissolution therein is in the solution.The present invention realizes the separation of three kinds of main constituents celluloses, hemicellulose and lignin in biomass.In addition, dissolution hemicellulose in the solution can through hydrolysis and add hydrogen and etc. be converted into tetrahydrofurfuryl alcohol to make up the solvent lost in reaction process, and tetrahydrofurfuryl alcohol solvent can be recycled by separation, have stronger application prospect.
Description
Technical field
The present invention relates to the comprehensive utilizations of biomass resource, more particularly, to fiber in a kind of solvent-thermal method separating biomass
The method of element, hemicellulose and lignin.
Background technique
A large amount of biomass is considered as potential renewable resource in widely distributed and nature, can be used for preparing combustion
Material, chemicals and material.Mainly by cellulose, hemicellulose and lignin, this three parts forms plant cell, they contain
Amount is respectively 30-50%, 15-25% and 15-30%.Interaction between lignin and cellulose and hemicellulose increases
The toughness of cell, and hinder the direct utilization of biomass.Therefore, separation lignocellulosic obtains cellulose, hemicellulose
It is of great significance with these three parts of lignin to the comprehensive utilization of biomass.
Initial period, biomass are mainly used for preparing the cellulose of high quality.Such as in sulfate process and soda pulping process
During, the cellulose of high quality can be obtained from sawdust for paper industry etc..But due to acid or alkaline condition
The obtained lignin structure of processing be largely changed, therefore, most of lignin is only burned and obtains thermal energy.
Then, the method for isolated high activity lignin is suggested, be using sawdust, under certain temperature and pressure, will be wooden
Quality is dissolved in the in the mixed solvent of organic solvent and water, and then precipitation and separation obtains the cellulose of high quality, but remaining
It include a large amount of hemicellulose and lignin in sawdust residue.Therefore, from biomass simultaneously isolated high quality fibre
Dimension element and lignin are faced with huge challenge.
The mixed solvent of tetrahydrofurfuryl alcohol and water can efficiently realize cellulose in biomass, hemicellulose and lignin
Separation, is conducive to its further trans-utilization.Meanwhile being prepared for the cellulose of higher degree and crystallinity and pure wooden
Element, and maintain a large amount of C-O key in lignin.Tetrahydrofurfuryl alcohol is reduced as a kind of high boiling organic solvent, its use
Requirement to consersion unit pressure boundary.And dissolve hemicellulose in the solution can through hydrolysis and add hydrogen and etc. turn
It turning to tetrahydrofurfuryl alcohol and makes up the solvent lost in reaction process, the tetrahydrofurfuryl alcohol and water in solution can separate recycling,
With stronger application prospect.
Summary of the invention
The main purpose of the present invention is to provide cellulose, hemicellulose and wood in a kind of solvent-thermal method separating biomass
The method of quality, the separation method is easy to operate, equipment investment is few, is conducive to the comprehensive high-efficiency for further realizing biomass resource
It utilizes.
To achieve the above object, the recyclable solvent tetrahydrofurfuryl alcohol based on hemicellulose that the present invention uses realizes biomass
Efficiently separate, scheme is as follows:
Biomass material, tetrahydrofurfuryl alcohol solvent and water are added in a kettle, after substitution gas, stirring and heating,
Reaction solution is separated, obtaining solid is cellulosic sections, and filtrate aqueous precipitation goes out solid, and lignin portion can be obtained in separation
Point, and hemicellulose is dissolved in dicyandiamide solution.And distillation separation further is carried out to the tetrahydrofurfuryl alcohol of in the mixed solvent and water.
Concrete technology method are as follows: biomass material, the tetrahydro chaff of -100 mesh of 2 mesh after comminution pretreatment are added in a kettle
Alcoholic solvent and water, wherein biomass material is sawdust and/or stalk, and stalk includes in corn stover, wheat stalk or straw
One or more, sawdust include one or more of beech, pine, birch or poplar, pretreated biology
The ratio between the additional amount and tetrahydrofurfuryl alcohol solvent of matter raw material and the total volume of water are 1g:(5-30) mL；Tetrahydrofurfuryl alcohol solvent and water
Volume ratio is (0.1-6): 1, reaction kettle is sealed, and with the air in nitrogen replacement reaction kettle, specifically: 15- is purged with nitrogen
It being maintained at after 20min under conditions of 1atm nitrogen, closes reaction kettle air inlet/outlet, stirring keeps 1-20h at 50-250 DEG C,
It is cooled to room temperature, is separated by filtration, obtain solid 1 and filtrate 1, solid 1 is washed with the mixed liquor of tetrahydrofurfuryl alcohol and water, wherein washing
The volume of mixed liquor used is (0.2-5) with the ratio between the volume of total volume for reacting tetrahydrofurfuryl alcohol solvent and water be added: 1, so
Drying solid 1 can obtain cellulose products afterwards；Water is added in filtrate 1 into above-mentioned steps, wherein the volume of water and anti-is added
Answering the ratio between total volume of middle solution is (0.5-5): after 1, magnetic agitation 0.5-5h, placing 6-20h, is separated by filtration, obtains solid 2
The solid 2 obtained with filtrate 2, washing separation obtains lignin product after drying solid 2；Hemicellulose is dissolved in above-mentioned steps
In in the filtrate 2 isolated；Air-distillation goes out the water in filtrate 2 at 100-120 DEG C, and further depressurizes at 80-130 DEG C
Tetrahydrofurfuryl alcohol solvent therein is distilled out, is recycled, hemicellulose can be obtained.
These three main components of cellulose, hemicellulose and lignin point in biomass can be realized using above-mentioned technique
From.After separation, the delignification of sawdust is up to 70-95%, and the yield of powder lignin reaches 65-90%, wherein lignin
Ratio shared by middle β-O-4 key is 30-60%.Cellulose purity is 80-100% in cellulose slurry, and the crystallinity of cellulose is
80-100%.The rate of recovery of tetrahydrofurfuryl alcohol reaches 70-85%, and the rate of recovery of water reaches 90-100%.
Compared with prior art route, the method for the present invention is had the advantages that
1. route of the present invention does not have corrosivity and tetrahydrofurfuryl alcohol boiling point is high, reaction pressure is low, therefore right
The requirement of consersion unit is lower, has biggish industrialization potential.
2. separation method of the invention is easy to operate, process cleans, cellulose in biomass, hemicellulose and wood are realized
The separation of quality lays a good foundation for the comprehensive high-efficiency utilization of biomass resource.
3. the hemicellulose that is dissolved in the present invention in solution through hydrolysis and add hydrogen and etc. be converted into tetrahydrofurfuryl alcohol, be
A kind of approach of green.
4. tetrahydrofurfuryl alcohol solvent and water used in the present invention can be separated and be recycled, production cost is reduced.
Specific embodiment
The following example will be helpful to understand the present invention, but the content of present invention is not limited thereto.
Embodiment 1
Beech is crushed, beech sawdust of the particle size between -100 mesh of 2 mesh after 20g is crushed then is weighed and is added
In reaction kettle, while 100mL tetrahydrofurfuryl alcohol and 150mL water is added, mechanical stirring mixes them thoroughly.Reaction kettle is sealed, nitrogen is used
Air-blowing is maintained under conditions of 1atm nitrogen after sweeping 15min, is closed air inlet/outlet, is used electric heating side under 600rpm mechanical stirring
Formula is warming up to 190 DEG C, reacts 400min.After reaction, the cooling reaction kettle of ice water stops stirring to room temperature, by reaction solution into
The isolated solid 1 of row and filtrate 1, solid 1 are washed with the mixed liquor of 80mL tetrahydrofurfuryl alcohol and 120mL water.And it will be after washing
The 105 DEG C of dry 12h in the vacuum tank that vacuum degree is -0.1MPa of solid 1 obtain cellulose.1.5L water is added into filtrate 1,
After stirring 2h, 10h is stood, is filtered, separation, and collect and obtain filtrate 2 and solid 2, solid 2 is washed 3 times, then in vacuum degree
Lignin is obtained for 40 DEG C in the vacuum tank of -0.1MPa dry 36h.Go out the water in filtrate 2 in 110 DEG C of air-distillations, goes forward side by side
One step is evaporated under reduced pressure out tetrahydrofurfuryl alcohol solvent at 110 DEG C, and is recycled, and after the distillation of filtrate 2 water outlet and tetrahydrofurfuryl alcohol solvent, remains
Remaining part is divided into hemicellulose, wherein the rate of recovery of tetrahydrofurfuryl alcohol and water can respectively reach 75.2% and 96.8%.
Using the analysis method of NREL/TP-510-42618, cellulose in beech sawdust, hemicellulose and wooden are determined
Cellulose content is respectively 47.0%, 20.9% and 21.1%, and the cellulose, hemicellulose and lignin in isolated cellulose slurry contain
Amount is respectively 90.4%, 5.3% and 2.8%.
According to the content analysis of three parts in biomass material and cellulose slurry, it can be deduced that beech is by tetrahydrofurfuryl alcohol
Processing, for delignification up to 86.7%, the yield of powder lignin reaches 78.1%, wherein in lignin shared by β-O-4 key
Ratio is 45.1%.Cellulose purity is 90.4% in cellulose slurry, and the crystallinity of cellulose is 90.2%.
Embodiment 2
Beech is crushed, beech sawdust of the particle size between -100 mesh of 2 mesh after 3g is crushed then is weighed and is added
In reaction kettle, while 10mL tetrahydrofurfuryl alcohol and 25mL water is added, magnetic agitation mixes them thoroughly.Reaction kettle is sealed, nitrogen is used
It is maintained under conditions of 1atm nitrogen after purging 20min, closes air inlet/outlet, use Electric heating under 600rpm magnetic agitation
200 DEG C are warming up to, 400min is reacted.After reaction, the cooling reaction kettle of ice water stops stirring, reaction solution is carried out to room temperature
Separation, obtains solid 1 and filtrate 1, and wash solid 1 with the mixed liquor of 10mL tetrahydrofurfuryl alcohol and 25mL water.By consolidating after washing
The 105 DEG C of dry 12h in the vacuum tank that vacuum degree is -0.1MPa of body 1 obtain cellulose.150mL water is added into filtrate 1,
After stirring 3h, 8h is stood, is filtered, separation, and collect and obtain filtrate 2 and solid 2, solid 2 is washed 5 times, then in vacuum degree
Lignin is obtained for 40 DEG C in the vacuum tank of -0.1MPa dry 36h.Go out the water in filtrate 2 in 110 DEG C of air-distillations, goes forward side by side
One step is evaporated under reduced pressure out tetrahydrofurfuryl alcohol solvent at 100 DEG C, and is recycled, and after the distillation of filtrate 2 water outlet and tetrahydrofurfuryl alcohol solvent, remains
Remaining part is divided into hemicellulose, wherein the rate of recovery of tetrahydrofurfuryl alcohol and water can respectively reach 73.1% and 98.2%.
Using the analysis method of NREL/TP-510-42618, cellulose in beech sawdust, hemicellulose and wooden are determined
Cellulose content is respectively 47.0%, 20.9% and 21.1%, and the cellulose, hemicellulose and lignin in isolated cellulose slurry contain
Amount is respectively 93.3%, 3.8% and 1.9%.
According to the content analysis of three parts in biomass material and cellulose slurry, it can be deduced that beech sawdust passes through tetrahydro chaff
The processing of alcohol, for delignification up to 91.0%, the yield of powder lignin reaches 82.1%, wherein β-O-4 key institute in lignin
The ratio accounted for is 40.1%.Cellulose purity is 93.3% in cellulose slurry, and the crystallinity of cellulose is 92.5%.
Embodiment 3
Beech is crushed, beech sawdust of the particle size between -100 mesh of 2 mesh after 25g is crushed then is weighed and is added
In reaction kettle, while 150mL tetrahydrofurfuryl alcohol and 130mL water is added, mechanical stirring mixes them thoroughly.Reaction kettle is sealed, nitrogen is used
Air-blowing is maintained under conditions of 1atm nitrogen after sweeping 15min, is closed air inlet/outlet, is used electric heating side under 600rpm mechanical stirring
Formula is warming up to 200 DEG C, reacts 350min.After reaction, the cooling reaction kettle of ice water stops stirring to room temperature, by reaction solution into
Row separation, obtains solid 1 and filtrate 1, and wash solid 1 with the mixed liquor of 150mL tetrahydrofurfuryl alcohol and 130mL water.After washing
Solid 1 in the vacuum tank that vacuum degree is -0.1MPa 105 DEG C of dry 12h be to obtain cellulose.1.5L is added into filtrate 1
Water after stirring 2h, stands 12h, filters, separation, and collects and obtain filtrate 2 and solid 2, solid 2 is washed 5 times, then in true
Reciprocal of duty cycle is that 40 DEG C of dry 36h obtain lignin in the vacuum tank of -0.1MPa.Go out the water in filtrate 2 in 110 DEG C of air-distillations,
And it further is evaporated under reduced pressure out tetrahydrofurfuryl alcohol solvent at 100 DEG C, and be recycled, the distillation of filtrate 2 water outlet and tetrahydrofurfuryl alcohol solvent
Afterwards, remainder is hemicellulose, wherein the rate of recovery of tetrahydrofurfuryl alcohol and water can respectively reach 70.5% and 99.0%.
Using the analysis method of NREL/TP-510-42618, cellulose in beech sawdust, hemicellulose and wooden are determined
Cellulose content is respectively 47.0%, 20.9% and 21.1%, and the cellulose, hemicellulose and lignin in isolated cellulose slurry contain
Amount is respectively 88.3%, 6.1% and 4.0%.
According to the content analysis of three parts in biomass material and cellulose slurry, it can be deduced that pine sawdust passes through Isosorbide-5-Nitrae-fourth
The processing of lactone, for delignification up to 81.0%, the yield of powder lignin reaches 73.6%, wherein β-O-4 key in lignin
Shared ratio is 49.6%.Cellulose purity is 88.3% in cellulose slurry, and the crystallinity of cellulose is 90.0%.
Embodiment 4
Beech is crushed, beech sawdust of the particle size between -100 mesh of 2 mesh after 30g is crushed then is weighed and is added
In reaction kettle, while 220mL tetrahydrofurfuryl alcohol and 150mL water is added, mechanical stirring mixes them thoroughly.Reaction kettle is sealed, nitrogen is used
Air-blowing is maintained under conditions of 1atm nitrogen after sweeping 15min, is closed air inlet/outlet, is used electric heating side under 600rpm mechanical stirring
Formula is warming up to 200 DEG C, reacts 500min.After reaction, the cooling reaction kettle of ice water stops stirring to room temperature, by reaction solution into
Row separation, obtains solid 1 and filtrate 1, and wash solid 1 with the mixed liquor of 220mL tetrahydrofurfuryl alcohol and 150mL water.After washing
Solid 1 in the vacuum tank that vacuum degree is -0.1MPa 105 DEG C of dry 12h be to obtain cellulose.1.5L is added into filtrate 1
Water after stirring 2h, stands 10h, filters, separation, and collects and obtain filtrate 2 and solid 2, solid 2 is washed 3 times, then in true
Reciprocal of duty cycle is that 40 DEG C of dry 36h obtain lignin in the vacuum tank of -0.1MPa.Go out the water in filtrate 2 in 110 DEG C of air-distillations,
And it further is evaporated under reduced pressure out tetrahydrofurfuryl alcohol solvent at 110 DEG C, and be recycled, the distillation of filtrate 2 water outlet and tetrahydrofurfuryl alcohol solvent
Afterwards, remainder is hemicellulose, wherein the rate of recovery of tetrahydrofurfuryl alcohol and water can respectively reach 72.5% and 98.3%.
Using the analysis method of NREL/TP-510-42618, cellulose in beech sawdust, hemicellulose and wooden are determined
Cellulose content is respectively 47.0%, 20.9% and 21.1%, and the cellulose, hemicellulose and lignin in isolated cellulose slurry contain
Amount is respectively 94.2%, 3.3% and 1.1%.
According to the content analysis of three parts in biomass material and cellulose slurry, it can be deduced that wheat stalk passes through tetrahydro chaff
The processing of alcohol, for delignification up to 94.8%, the yield of powder lignin reaches 84.3%, wherein β-O-4 key institute in lignin
The ratio accounted for is 36.6%.Cellulose purity is 94.2% in cellulose slurry, and the crystallinity of cellulose is 98.3%.
The experimental procedure of embodiment 5 is same as Example 1, needs for biomass material to be changed to corn stover, reaction temperature
It is changed to 150 DEG C.
The experimental procedure of embodiment 6 is same as Example 2, needs for biomass material to be changed to corn stover, reaction temperature
It is changed to 190 DEG C.
The experimental procedure of embodiment 7 is same as Example 3, needs for biomass material to be changed to corn stover, reaction temperature
210 DEG C are changed to, the reaction time is changed to 300min.
The experimental procedure of embodiment 8 is same as Example 4, needs for biomass material to be changed to corn stover, reaction temperature
It is changed to 210 DEG C.
The experimental procedure of embodiment 9 is same as Example 1, needs for biomass material to be changed to wheat stalk, reaction temperature
180 DEG C are changed to, the reaction time is changed to 200min.
The experimental procedure of embodiment 10 is same as Example 2, needs for biomass material to be changed to wheat stalk, reaction time
It is changed to 200min.
The experimental procedure of embodiment 11 is same as Example 4, needs for biomass material to be changed to wheat stalk, reaction time
It is changed to 400min.
The experimental procedure of embodiment 12 is same as Example 1, needs biomass material being changed to straw.
The experimental procedure of embodiment 13 is same as Example 3, needs for biomass material to be changed to straw, the reaction time is changed to
400min。
The experimental procedure of embodiment 14 is same as Example 4, needs for biomass material to be changed to straw, reaction temperature is changed to
210 DEG C, the reaction time is changed to 400min.
The experimental procedure of embodiment 15 is same as Example 1, needs for biomass material to be changed to pine, reaction temperature is changed to
200 DEG C, the reaction time is changed to 350min.
The experimental procedure of embodiment 16 is same as Example 3, needs for biomass material to be changed to pine, reaction temperature is changed to
220℃。
The experimental procedure of embodiment 17 is same as Example 4, needs for biomass material to be changed to pine, reaction temperature is changed to
210℃。
The experimental procedure of embodiment 18 is same as Example 2, needs for biomass material to be changed to birch, reaction temperature is changed to
180 DEG C, the reaction time is changed to 500min.
The experimental procedure of embodiment 19 is same as Example 3, needs for biomass material to be changed to birch, reaction temperature is changed to
190 DEG C, the reaction time is changed to 500min.
The experimental procedure of embodiment 20 is same as Example 4, needs biomass material being changed to birch.
The experimental procedure of embodiment 21 is same as Example 1, needs for biomass material to be changed to poplar, reaction temperature is changed to
210℃。
The experimental procedure of embodiment 22 is same as Example 2, needs for biomass material to be changed to poplar, reaction temperature is changed to
210 DEG C, the reaction time is changed to 500min.
The experimental procedure of embodiment 23 is same as Example 4, needs for biomass material to be changed to poplar, reaction temperature is changed to
220 DEG C, the reaction time is changed to 600min.
Specific experiment condition and result summary are shown in Table 1 in embodiment.
1. experiment condition of table and result are summarized
Claims (8)
1. a kind of method of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass, it is characterised in that:
Biomass material is carried out comminution pretreatment using pulverizer by step 1.；
In a kettle, the biomass material and tetrahydrofurfuryl alcohol solvent and water of crushing obtained in addition step 1 are close for step 2.
Reaction kettle is sealed, stirring keeps 1-20h at 50-250 DEG C, is cooled to room temperature, be separated by filtration, obtain solid 1 and filtrate 1, with four
The mixed liquor of hydrogen chaff alcohol and water washs solid 1, and cellulose products can be obtained by then drying solid 1；
Step 3. is added water into the filtrate 1 in step 2, after magnetic agitation 0.5-5h, places 6-20h, is separated by filtration, consolidate
Body 2 and filtrate 2, the solid 2 that washing separation obtains obtain lignin product after drying solid 2；
Step 4. hemicellulose is dissolved in the filtrate 2 that step 3 is isolated；
Step 5. air-distillation at 100-120 DEG C goes out the water in filtrate 2, and is further evaporated under reduced pressure out it at 80-130 DEG C
In tetrahydrofurfuryl alcohol solvent, recycled, hemicellulose can be obtained.
2. method according to claim 1, it is characterised in that: in step 1, block is cut into after biomass material is dried, is used
Pulverizer is crushed, and the particle size of smashed biomass material is between -100 mesh of 2 mesh.
3. method according to claim 1, it is characterised in that: in step 1, biomass is sawdust and/or stalk, and stalk includes
One or more of corn stover, wheat stalk or straw, sawdust include one in beech, pine, birch or poplar
Kind is two or more.
4. method according to claim 1, it is characterised in that: in step 2, in reaction kettle, pretreated biomass material
Additional amount and the ratio between the total volume of tetrahydrofurfuryl alcohol solvent and water be 1g:(5-30) mL；The volume ratio of tetrahydrofurfuryl alcohol solvent and water
For (0.1-6): 1.
5. method according to claim 1, it is characterised in that: in step 2, wash the volume of mixed liquor used with react added by
Entering the ratio between volume of total volume of tetrahydrofurfuryl alcohol solvent and water is (0.2-5): 1.
6. method according to claim 1, it is characterised in that: in step 2, used in nitrogen replacement reaction kettle after sealing reaction kettle
Air, specifically: with nitrogen purge 15-20min after be maintained at 1atm nitrogen under conditions of, close reaction kettle air inlet/outlet.
7. method according to claim 1, it is characterised in that: in step 3, be added into filtrate 1 volume of water with react
The ratio between total volume of solution is (0.5-5): 1.
8. method according to claim 1, it is characterised in that: in step 3, washing solid 2 is to be washed with deionized water 2-7 times.
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| CN112442924A (en) * | 2019-09-03 | 2021-03-05 | 中国科学院大连化学物理研究所 | Method for preparing high-hardness environment-friendly material by using protogenic plant biomass as raw material |
| CN112442924B (en) * | 2019-09-03 | 2022-06-14 | 中国科学院大连化学物理研究所 | Method for preparing high-hardness environment-friendly material by using protogenic plant biomass as raw material |
| CN113024492A (en) * | 2021-03-25 | 2021-06-25 | 北京林业大学 | Method for comprehensively utilizing corn straws based on tetrahydrofurfuryl alcohol/water |
| CN113115969A (en) * | 2021-04-02 | 2021-07-16 | 中国烟草总公司郑州烟草研究院 | Method for reducing lignin content in tobacco stems |
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Application publication date: 20190521 |