CN109438724A - The method and its application of lignin in a kind of extraction lignocellulosic - Google Patents
The method and its application of lignin in a kind of extraction lignocellulosic Download PDFInfo
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- CN109438724A CN109438724A CN201811429456.4A CN201811429456A CN109438724A CN 109438724 A CN109438724 A CN 109438724A CN 201811429456 A CN201811429456 A CN 201811429456A CN 109438724 A CN109438724 A CN 109438724A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The present invention relates to a kind of methods of lignin in extraction lignocellulosic, include the following steps: to crush the ball milling together with pearl powder of the lignocellulosic material after drying, extractant is added into the mixture after ball milling to be extracted, passes through addition supercritical CO before extraction and in extraction process2It is 10Mpa ~ 30Mpa to control extracting pressure, extract liquor is evaporated to obtain wooden cellulose crystal.Invention additionally discloses the applications to the method for lignin in the extraction lignocellulosic.The present invention is that a kind of environmental protection, economy, reaction condition are suitble to the method for the cleaning of biological material, efficient purifying lignin.
Description
Technical field
The invention belongs to lignin preparation technical field, in particular to wood in a kind of lignocellulosic for extracting biomaterial
The method of quality.
Background technique
Lignocellulose biomass is resourceful, repeats regeneration, has prepared fuels and chemicals currently with biomass
As research hotspot.Lignocellulosic is made of cellulose, hemicellulose, lignin, wherein the lignin conduct of reticular structure
Support frame surrounds and reinforces cellulose and hemicellulose, and for the content of lignin between 15-30%, energy storage is even more height
It is the important source material source of potential sustainable energy and bulk chemical up to 40% or more.
Lignin is one of the main component for constituting plant skeleton, and the whole world is regenerated by the ecological circulation chain of plant every year
About 50,000,000,000 tons of lignin, be second largest renewable, the biodegradable resource of cellulose is only second in nature, and from
The aromatic series natural polymer of unique environment close friend in right boundary.Lignin may be used as important industrial chemicals.
Important composition ingredient one of of the lignin as plant cell wall, is a kind of reproducible biomass resource.Due to
It has energy more higher than cellulose, therefore becomes one of the primary raw material of current research biomass energy.Currently on the market
Industrial lignin is mainly derived from papermaking wastewater, secondly can also generate a large amount of wood during Wooden Biomass alcohol prepared by fermenting
Quality.However, lignin is far from being fully utilized in chemical industry, it is primarily due to lignin separation in prior art
Extraction process is complicated, at high cost or seriously polluted.
At this stage there are many ways to lignocellulosic pretreatment separating lignin, for example, it is organic solvent extraction, inorganic
Alkali process, mineral acid treatment, organic acidic treatment etc., and then obtain the lignin raw material of a variety of differing chemical properties.Wherein
Organic solvent method is considered as the technology of best separating lignin.But the method it is isolated lignin molecule amount it is low, it is living
Property height is unstable, and often operates at high temperature under high pressure, it is therefore desirable to high temperature high voltage resistant equipment.Simultaneously in lignin extraction process
In need hydrochloric acid or sulfuric acid is catalyzed, therefore be unfavorable for the recycling of organic solvent.Traditional chemical pulp processes benefit
Effectively lignin extraction can be come out with chemicals such as highly basic, sulfate, but this traditional pulping process condition is harsh,
It will cause environmental pollution, and isolated alkali lignin, because of height polycondensation, active function groups are lost and are difficult to be utilized.It passes
The ionic liquid of system, especially glyoxaline ion liquid can efficiently extract the lignin in biomass material, but because of it
Potential bio-toxicity, viscosity is big, separating lignin temperature is high, and high cost and poor biological degradability make its development
It is restricted.Therefore we need to develop a kind of environmental protection, economy, reaction condition are suitble to biomass clean, efficiently purify
The method of lignin is of great significance.
Summary of the invention
Technical problem to be solved by the present invention lies in, provide it is a kind of extraction lignocellulosic in lignin method and its
Using using lignocellulosic as raw material, to a series of processing of lignocellulosic material progress, from treated, lignocellulosic is former
Lignin is extracted in material, obtains the lignin of high-purity, is that a kind of environmental protection, economy, reaction condition are suitble to the clear of biological material
The method of clean, efficient purifying lignin.
The invention is realized in this way providing a kind of method for extracting lignin in lignocellulosic, include the following steps:
By lignocellulosic material of the crushing after dry ball milling together with pearl powder, extractant is added into the mixture after ball milling and carries out
Extraction passes through addition supercritical CO before extraction and in extraction process2It is 10Mpa ~ 30Mpa to control extracting pressure, to extraction
Liquid is evaporated to obtain wooden cellulose crystal.
Further, the lignocellulosic material includes corn stover, corncob, agriculture and forestry organic waste material, sugarcane, wheat,
At least one of sugar grass.
Further, the extractant is the mixed solvent of Tween 80 and water, or molten for the mixing of polyethylene glycol and water
Agent.
Further, in the in the mixed solvent of Tween 80 and water, the mass ratio of Tween 80 and water are as follows: 1:1~1:9；Poly-
The mass ratio of the in the mixed solvent of ethylene glycol and water, polyethylene glycol and water are as follows: 1:5~1:10.
Further, the method for extracting lignin in lignocellulosic includes the following steps:
(1) lignocellulosic material crushes: using lignocellulosic as raw material, lignocellulosic material being carried out to crush dry place
Reason；
(2) lignocellulosic material is mixed with pearl powder: by smashed lignocellulosic material and pearl powder according to quality into
Row proportion, lignocellulosic material: pearl powder=1:1~1:5 obtains the mixture of lignocellulosic and pearl powder；
(3) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: to the mixture of lignocellulosic and pearl powder
Ball milling is carried out using ball mill, obtains the ball milling powder of lignocellulosic and pearl powder, wherein the partial size of lignocellulosic maintains
200 mesh ~ 400 mesh；
(4) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g lignocellulosic in step (3) and treasure
The ball milling powder of pearl is fitted into extraction kettle；
(5) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1~1:9, and it is spare；
(6) heats up to extraction kettle: heating to extraction kettle, controls 40 DEG C ~ 60 DEG C of temperature of extraction kettle；
(7) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 10Mpa ~ 30Mpa；
(8) extractant that step (5) configure, flow 0.1ml/min ~ 0.5ml/ of extractant static extracting: is added to extraction kettle
Min is passed through time 0.5h ~ 2h, static extracting time 0.5h ~ 2h；
(9) dynamic extraction: after the completion of step (8) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.1ml/min
~ 0.5ml/min, dynamic extraction time 1h ~ 3h, is constantly passed through supercritical CO to extraction kettle2, and extractant is added to extraction kettle
2 times ~ 5 times, control extraction kettle pressure is 10Mpa ~ 30Mpa；
(10) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (9), temperature is controlled at 50 DEG C ~ 70 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.09 Mpa ~ 0.1Mpa.
A kind of foregoing answering for the method for lignin in lignocellulosic is extracted the invention is realized in this way providing
With the method for lignin is applied in food industry or medical industry or biological environmental production industry in the extraction lignocellulosic.
Compared with prior art, the method and its application for extracting lignin in lignocellulosic of the invention, with wooden fibre
Dimension element is raw material, is dried by crushing, and weighs a certain amount of lignocellulosic material and pearl powder is proportionally placed on ball
In grinding machine, for a period of time, the lignocellulosic after ball milling is placed in extraction kettle for ball milling, prepare a certain proportion of Tween 80 with
Water extractant, heats up to extraction kettle, and supercritical CO is added2Extracting pressure is controlled, after temperature, pressure reaches and to stablize, is led to
It is a certain amount of to enter extractant, static extracting for a period of time, is passed through extractant and supercritical CO again2When carrying out one section of dynamic extraction
Between, extractant is passed through by using syringe pump, the number for being passed through extractant is 2 ~ 5 times, is rotated to extract liquor, to obtain
Wooden cellulose crystal.
The method and its application of lignin have the following characteristics that in extraction lignocellulosic of the invention
1. processing of the ball mill to lignocellulosic is a kind of preconditioning technique of green high-efficient, so that lignin is easier to mention
It takes；
2. using Tween 80 and water as extractant, the lignin of preparation has environmentally protective, non-corrosive excellent performance,
Lignin extraction rate reaches 95% ~ 99.8%；
3. the solvent for extracting lignin can be recycled, is recycled, reduction production cost is low, practical, easily realizes industry
Change；
4. supercritical CO2Technology using environmentally protective, extract the more efficient of lignin, shorten total extraction time 2h ~ 5h,
Efficiency improves 60% ~ 80%, and the purity of the lignin extracted is higher, and the purity of lignin reaches 95% ~ 99.65%, extraction
Temperature is reduced to 40 DEG C ~ 60 DEG C, reduces energy consumption 30% ~ 50%；
5. Rotary Evaporators separating lignin is used, it is easy to operate, it is at low cost, lignin structure will not be destroyed, while obtaining
Lignin solvent's residual is less, and dissolvent residual is nontoxic less than 1% in lignin.
Specific embodiment
In order to which technical problems, technical solutions and advantages to be solved are more clearly understood, tie below
Embodiment is closed, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to solve
The present invention is released, is not intended to limit the present invention.
The present invention extracts the preferred embodiment of the method for lignin in lignocellulosic, includes the following steps: to crush dry
Lignocellulosic material after the dry ball milling together with pearl powder is added extractant into the mixture after ball milling and is extracted, extracted
Pass through addition supercritical CO before taking and in extraction process2It is 10Mpa ~ 30Mpa to control extracting pressure, extract liquor is steamed
Hair obtains wooden cellulose crystal.The lignocellulosic material includes corn stover, corncob, agriculture and forestry organic waste material, sugarcane, wheat,
At least one of sugar grass.
The extractant is the mixed solvent of Tween 80 and water, or the mixed solvent for polyethylene glycol and water.In tween
80 with the in the mixed solvent of water, the mass ratio of Tween 80 and water are as follows: 1:1~1:9.In the in the mixed solvent of polyethylene glycol and water,
The mass ratio of polyethylene glycol and water are as follows: 1:5~1:10.
Specifically, the method for extracting lignin in lignocellulosic includes the following steps:
(1) lignocellulosic material crushes: using lignocellulosic as raw material, lignocellulosic material being carried out to crush dry place
Reason.
(2) lignocellulosic material is mixed with pearl powder: by smashed lignocellulosic material and pearl powder according to matter
Amount is matched, and lignocellulosic material: pearl powder=1:1~1:5 obtains the mixture of lignocellulosic and pearl powder.
(3) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: mixing to lignocellulosic and pearl powder
It closes object and carries out ball milling using ball mill, Ball-milling Time 12h ~ 48h obtains the ball milling powder of lignocellulosic and pearl powder, wherein wood
The partial size of matter cellulose maintains 200 mesh ~ 400 mesh.
(4) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g lignocellulosic in step (3)
It is fitted into extraction kettle with the ball milling powder of pearl.
(5) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1~1:9, and it is spare.
(6) heats up to extraction kettle: heating to extraction kettle, controls 40 DEG C ~ 60 DEG C of temperature of extraction kettle.
(7) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 10Mpa ~ 30Mpa.
(8) static extracting: being added the extractant that step (5) configure to extraction kettle, and the flow 0.1ml/min of extractant ~
0.5ml/min is passed through time 0.5h ~ 2h, static extracting time 0.5h ~ 2h.
(9) dynamic extraction: after the completion of step (8) static extracting, then dynamic extraction is carried out, the flow of extractant is
0.1ml/min ~ 0.5ml/min, dynamic extraction time 1h ~ 3h, is constantly passed through supercritical CO to extraction kettle2, and to extraction kettle
It is added extractant 2 times ~ 5 times, control extraction kettle pressure is 10Mpa ~ 30Mpa.
Different from common dynamic extraction method, the present invention is during dynamic extraction, in addition to constantly logical to extraction kettle
Enter supercritical CO2Outside, constantly supplement is added extractant 2 times ~ 5 times also into extraction kettle, and purpose is not only to increase in extraction kettle
The capacity of extractant, but also the activity of extractant in extraction kettle is further maintained, improve its extracting power.
(10) extract liquor evaporates: carrying out rotary evaporation to the extract liquor after the completion of step (9), temperature is controlled 50 DEG C ~ 70
DEG C, vacuum degree control obtains wooden cellulose crystal after dry in 0.09 Mpa ~ 0.1Mpa.It is measured in obtained wooden cellulose crystal
Lignin purity 95% ~ 99.6%, the purity is high of lignin.
Invention additionally discloses a kind of foregoing application for extracting the method for lignin in lignocellulosic, extraction wood
The method of lignin is applied in food industry or medical industry or biological environmental production industry in matter cellulose.
The method for extracting lignin in lignocellulosic of the invention is further illustrated combined with specific embodiments below.
Embodiment 1.
The method of lignin, the embodiment include the following steps: in the first extraction lignocellulosic of the present invention
(11) lignocellulosic material crushes: using corn stover as raw material, corn stalk raw material being carried out crushing drying process.
(12) lignocellulosic material is mixed with pearl powder: by smashed corn stalk raw material and pearl powder according to matter
Amount is matched, and corn stalk raw material: pearl powder=1:1 obtains the mixture of corn stover and pearl powder.
(13) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: mixing to corn stover and pearl powder
It closes object and carries out ball milling using ball mill, Ball-milling Time 12h obtains the ball milling powder of corn stover and pearl powder, wherein corn stover
Partial size maintain 200 mesh.
(14) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g corn stover in step (13)
It is fitted into extraction kettle with the ball milling powder of pearl.
(15) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1, and it is spare.
(16) heats up to extraction kettle: heating to extraction kettle, controls 40 DEG C of temperature of extraction kettle.
(17) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 10Mpa.
(18) static extracting: the extractant configured to extraction kettle addition step (15), the flow 0.1ml/min of extractant,
It is passed through time 0.5h, static extracting time 0.5hh.
(19) dynamic extraction: after the completion of step (18) static extracting, then dynamic extraction is carried out, the flow of extractant is
0.1ml/min, dynamic extraction time 1h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 2 times to extraction kettle,
Control extraction kettle pressure is 10Mpa.
(110) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (19), temperature is controlled at 50 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.09 Mpa.
Embodiment 2.
Second of method for extracting lignin in lignocellulosic of the present invention, the embodiment include the following steps:
(21) lignocellulosic material crushes: using corncob as raw material, corn core raw material being carried out crushing drying process.
(22) lignocellulosic material is mixed with pearl powder: by smashed corn core raw material and pearl powder according to quality
Matched, corn core raw material: pearl powder=1:5 obtains the mixture of corncob and pearl powder.
(23) carries out ball-milling treatment: the mixing to corncob and pearl powder to the mixture of lignocellulosic and pearl powder
Object carries out ball milling using ball mill, and Ball-milling Time 48h obtains the ball milling powder of corncob and pearl powder, wherein the partial size of corncob
Maintain 400 mesh.
(24) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weigh 50g corncob in step (23) with
The ball milling powder of pearl is fitted into extraction kettle.
(25) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1, and it is spare.
(26) heats up to extraction kettle: heating to extraction kettle, controls the temperature 60 C of extraction kettle.
(27) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 30Mpa.
(28) static extracting: the extractant configured to extraction kettle addition step (25), the flow 0.5ml/min of extractant,
It is passed through time 1h, static extracting time 2h.
(29) dynamic extraction: after the completion of step (28) static extracting, then dynamic extraction is carried out, the flow of extractant is
0.5ml/min, dynamic extraction time 3h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 5 times to extraction kettle,
Control extraction kettle pressure is 30Mpa.
(210) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (29), temperature is controlled at 70 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.1Mpa.
Embodiment 3.
The method of lignin, the embodiment include the following steps: in the third extraction lignocellulosic of the present invention
(31) lignocellulosic material crushes: using agriculture and forestry organic waste material as raw material, agriculture and forestry organic waste material raw material being carried out to crush dry place
Reason.
(32) lignocellulosic material is mixed with pearl powder: by smashed agriculture and forestry organic waste material raw material and pearl powder according to
Quality is matched, agriculture and forestry organic waste material raw material: pearl powder=1:3 obtains the mixture of agriculture and forestry organic waste material and pearl powder.
(33) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: to agriculture and forestry organic waste material and pearl powder
Mixture carries out ball milling using ball mill, and Ball-milling Time for 24 hours, obtains the ball milling powder of agriculture and forestry organic waste material and pearl powder, wherein agricultural
The partial size of waste maintains 300 mesh.
(34) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: the 50g agricultural weighed in step (33) are discarded
Object and the ball milling powder of pearl are fitted into extraction kettle.
(35) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:9, and it is spare.
(36) heats up to extraction kettle: heating to extraction kettle, controls the temperature 50 C of extraction kettle.
(37) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 20Mpa.
(38) static extracting: the extractant configured to extraction kettle addition step (35), the flow 0.3ml/min of extractant,
It is passed through time 0.5h, static extracting time 2h.
(39) dynamic extraction: after the completion of step (38) static extracting, then dynamic extraction is carried out, the flow of extractant is
0.3ml/min, dynamic extraction time 2h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 3 times to extraction kettle,
Control extraction kettle pressure is 20Mpa.
(310) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (39), temperature is controlled at 60 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.09Mpa.
Embodiment 4.
The 4th kind of method for extracting lignin in lignocellulosic of the present invention, the embodiment include the following steps:
(41) lignocellulosic material crushes: using sugarcane as raw material, sugarcane raw material being carried out crushing drying process.
(42) lignocellulosic material is mixed with pearl powder: by smashed sugarcane raw material and pearl powder according to quality into
Row proportion, sugarcane raw material: pearl powder=1:2 obtains the mixture of sugarcane and pearl powder.
(43) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: to the mixture of sugarcane and pearl powder
Ball milling is carried out using ball mill, Ball-milling Time 48h obtains the ball milling powder of sugarcane and pearl powder, wherein the partial size of lignocellulosic
Maintain 400 mesh.
(44) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g sugarcane in step (43) and treasure
The ball milling powder of pearl is fitted into extraction kettle.
(45) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:5, and it is spare.
(46) heats up to extraction kettle: heating to extraction kettle, controls the temperature 60 C of extraction kettle.
(47) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 25Mpa.
(48) static extracting: the extractant configured to extraction kettle addition step (45), the flow 0.3ml/min of extractant,
It is passed through time 1h, static extracting time 2h.
(49) dynamic extraction: after the completion of step (48) static extracting, then dynamic extraction is carried out, the flow of extractant is
0.3ml/min, dynamic extraction time 3h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 4 times to extraction kettle,
Control extraction kettle pressure is 25Mpa.
(410) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (49), temperature is controlled at 50 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.1Mpa.
The content for measuring lignin in the finally prepd wooden cellulose crystal of the various embodiments described above, obtains the wooden of embodiment 1
Plain purity 95%, the lignin purity 99.6% of embodiment 2, the measurement lignin purity 97.9% of embodiment 3, embodiment 4 it is wooden
Plain purity 98.9%., it is with high purity, realize technical effect of the invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of method for extracting lignin in lignocellulosic, which comprises the steps of: after drying being crushed
Lignocellulosic material ball milling together with pearl powder, into the mixture after ball milling be added extractant extracted, extraction before with
And by the way that supercritical CO is added in extraction process2It is 10Mpa ~ 30Mpa to control extracting pressure, extract liquor is evaporated to obtain
Wooden cellulose crystal.
2. extracting the method for lignin in lignocellulosic as described in claim 1, which is characterized in that the lignocellulosic
Raw material includes corn stover, corncob, agriculture and forestry organic waste material, sugarcane, wheat, at least one of sugar grass.
3. extracting the method for lignin in lignocellulosic as claimed in claim 2, which is characterized in that the extractant is to spit
The mixed solvent of temperature 80 and water, or the mixed solvent for polyethylene glycol and water.
4. extracting the method for lignin in lignocellulosic as claimed in claim 3, which is characterized in that in Tween 80 and water
The mass ratio of in the mixed solvent, Tween 80 and water are as follows: 1:1~1:9；In the in the mixed solvent of polyethylene glycol and water, polyethylene glycol
With the mass ratio of water: 1:5~1:10.
5. extracting the method for lignin in lignocellulosic as claimed in claim 4, which is characterized in that described to extract wooden fibre
The method of lignin includes the following steps: in dimension element
(1) lignocellulosic material crushes: using lignocellulosic as raw material, lignocellulosic material being carried out to crush dry place
Reason；
(2) lignocellulosic material is mixed with pearl powder: by smashed lignocellulosic material and pearl powder according to quality
Matched, lignocellulosic material: pearl powder=1:1~1:5 obtains the mixture of lignocellulosic and pearl powder；
(3) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: to the mixture of lignocellulosic and pearl powder
Ball milling is carried out using ball mill, obtains the ball milling powder of lignocellulosic and pearl powder, wherein the partial size of lignocellulosic maintains
200 mesh ~ 400 mesh；
(4) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g lignocellulosic in step (3) and treasure
The ball milling powder of pearl is fitted into extraction kettle；
(5) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1~1:9, and it is spare；
(6) heats up to extraction kettle: heating to extraction kettle, controls 40 DEG C ~ 60 DEG C of temperature of extraction kettle；
(7) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 10Mpa ~ 30Mpa；
(8) extractant that step (5) configure, flow 0.1ml/min ~ 0.5ml/ of extractant static extracting: is added to extraction kettle
Min is passed through time 0.5h ~ 2h, static extracting time 0.5h ~ 2h；
(9) dynamic extraction: after the completion of step (8) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.1ml/min
~ 0.5ml/min, dynamic extraction time 1h ~ 3h, is constantly passed through supercritical CO to extraction kettle2, and extractant is added to extraction kettle
2 times ~ 5 times, control extraction kettle pressure is 10Mpa ~ 30Mpa；
(10) extract liquor evaporates: rotary evaporation is carried out to the extract liquor after the completion of step (9), temperature is controlled at 50 DEG C ~ 70 DEG C,
Vacuum degree control obtains wooden cellulose crystal after dry in 0.09 Mpa ~ 0.1Mpa.
6. extracting the method for lignin in lignocellulosic as claimed in claim 5, which is characterized in that described to extract wooden fibre
The method of lignin includes the following steps: in dimension element
(11) lignocellulosic material crushes: using corn stover as raw material, corn stalk raw material being carried out crushing drying process；
(12) lignocellulosic material is mixed with pearl powder: by smashed corn stalk raw material and pearl powder according to quality into
Row proportion, corn stalk raw material: pearl powder=1:1 obtains the mixture of corn stover and pearl powder；
(13) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: to the mixture of corn stover and pearl powder
Ball milling is carried out using ball mill, Ball-milling Time 12h obtains the ball milling powder of corn stover and pearl powder, wherein the grain of corn stover
Diameter maintains 200 mesh；
(14) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g corn stover in step (13) and treasure
The ball milling powder of pearl is fitted into extraction kettle；
(15) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1, and it is spare；
(16) heats up to extraction kettle: heating to extraction kettle, controls 40 DEG C of temperature of extraction kettle；
(17) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 10Mpa；
(18) static extracting: the extractant that step (15) configure is added to extraction kettle, the flow 0.1ml/min of extractant is passed through
Time 0.5h, static extracting time 0.5hh；
(19) dynamic extraction: after the completion of step (18) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.1ml/
Min, dynamic extraction time 1h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 2 times to extraction kettle, control extraction
Taking kettle pressure is 10Mpa；
(110) extract liquor evaporates: carrying out rotary evaporation to the extract liquor after the completion of step (19), temperature control is at 50 DEG C, vacuum
Degree control obtains wooden cellulose crystal after dry in 0.09 Mpa.
7. extracting the method for lignin in lignocellulosic as claimed in claim 5, which is characterized in that described to extract wooden fibre
The method of lignin includes the following steps: in dimension element
(21) lignocellulosic material crushes: using corncob as raw material, corn core raw material being carried out crushing drying process；
(22) lignocellulosic material is mixed with pearl powder: smashed corn core raw material and pearl powder are carried out according to quality
Proportion, corn core raw material: pearl powder=1:5 obtains the mixture of corncob and pearl powder；
(23) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: making to the mixture of corncob and pearl powder
Ball milling is carried out with ball mill, Ball-milling Time 48h obtains the ball milling powder of corncob and pearl powder, wherein the partial size of corncob maintains
In 400 mesh；
(24) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing the 50g corncob in step (23) and pearl
Ball milling powder be fitted into extraction kettle；
(25) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:1, and it is spare；
(26) heats up to extraction kettle: heating to extraction kettle, controls the temperature 60 C of extraction kettle；
(27) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 30Mpa；
(28) static extracting: the extractant that step (25) configure is added to extraction kettle, the flow 0.5ml/min of extractant is passed through
Time 1h, static extracting time 2h；
(29) dynamic extraction: after the completion of step (28) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.5ml/
Min, dynamic extraction time 3h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 5 times to extraction kettle, control extraction
Taking kettle pressure is 30Mpa；
(210) extract liquor evaporates: carrying out rotary evaporation to the extract liquor after the completion of step (29), temperature control is at 70 DEG C, vacuum
Degree control obtains wooden cellulose crystal after dry in 0.1Mpa.
8. extracting the method for lignin in lignocellulosic as claimed in claim 5, which is characterized in that described to extract wooden fibre
The method of lignin includes the following steps: in dimension element
(31) lignocellulosic material crushes: using agriculture and forestry organic waste material as raw material, agriculture and forestry organic waste material raw material being carried out to crush dry place
Reason；
(32) lignocellulosic material is mixed with pearl powder: by smashed agriculture and forestry organic waste material raw material and pearl powder according to quality
Matched, agriculture and forestry organic waste material raw material: pearl powder=1:3 obtains the mixture of agriculture and forestry organic waste material and pearl powder；
(33) carries out ball-milling treatment: the mixing to agriculture and forestry organic waste material and pearl powder to the mixture of lignocellulosic and pearl powder
Object carries out ball milling using ball mill, and Ball-milling Time for 24 hours, obtains the ball milling powder of agriculture and forestry organic waste material and pearl powder, wherein agricultural are discarded
The partial size of object maintains 300 mesh；
(34) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weigh 50g agriculture and forestry organic waste material in step (33) with
The ball milling powder of pearl is fitted into extraction kettle；
(35) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:9, and it is spare；
(36) heats up to extraction kettle: heating to extraction kettle, controls the temperature 50 C of extraction kettle；
(37) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 20Mpa；
(38) static extracting: the extractant that step (35) configure is added to extraction kettle, the flow 0.3ml/min of extractant is passed through
Time 0.5h, static extracting time 2h；
(39) dynamic extraction: after the completion of step (38) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.3ml/
Min, dynamic extraction time 2h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 3 times to extraction kettle, control extraction
Taking kettle pressure is 20Mpa；
(310) extract liquor evaporates: carrying out rotary evaporation to the extract liquor after the completion of step (39), temperature control is at 60 DEG C, vacuum
Degree control obtains wooden cellulose crystal after dry in 0.09Mpa.
9. extracting the method for lignin in lignocellulosic as claimed in claim 5, which is characterized in that described to extract wooden fibre
The method of lignin includes the following steps: in dimension element
(41) lignocellulosic material crushes: using sugarcane as raw material, sugarcane raw material being carried out crushing drying process；
(42) lignocellulosic material is mixed with pearl powder: smashed sugarcane raw material and pearl powder are matched according to quality
Than sugarcane raw material: pearl powder=1:2 obtains the mixture of sugarcane and pearl powder；
(43) carries out ball-milling treatment to the mixture of lignocellulosic and pearl powder: using the mixture of sugarcane and pearl powder
Ball mill carries out ball milling, and Ball-milling Time 48h obtains the ball milling powder of sugarcane and pearl powder, wherein the partial size of lignocellulosic maintains
In 400 mesh；
(44) ball milling powder of lignocellulosic and pearl powder is fitted into extraction kettle: weighing 50g sugarcane in step (43) and pearl
Ball milling powder is fitted into extraction kettle；
(45) configures extractant: the extractant of Tween 80 and water is prepared, Tween 80: water quality ratio=1:5, and it is spare；
(46) heats up to extraction kettle: heating to extraction kettle, controls the temperature 60 C of extraction kettle；
(47) boosts to extraction kettle: being passed through supercritical CO to extraction kettle2, control extraction kettle pressure is 25Mpa；
(48) static extracting: the extractant that step (45) configure is added to extraction kettle, the flow 0.3ml/min of extractant is passed through
Time 1h, static extracting time 2h；
(49) dynamic extraction: after the completion of step (48) static extracting, then carrying out dynamic extraction, and the flow of extractant is 0.3ml/
Min, dynamic extraction time 3h, is constantly passed through supercritical CO to extraction kettle2, and be added extractant 4 times to extraction kettle, control extraction
Taking kettle pressure is 25Mpa；
(410) extract liquor evaporates: carrying out rotary evaporation to the extract liquor after the completion of step (49), temperature control is at 50 DEG C, vacuum
Degree control obtains wooden cellulose crystal after dry in 0.1Mpa.
10. a kind of application for extracting the method for lignin in lignocellulosic as in one of claimed in any of claims 1 to 9,
It is characterized in that, the method for lignin is applied to food industry or medical industry or biological environmental production in the extraction lignocellulosic
In industry.
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