CN109722932A - A method of extracting agricultural stalk class waste cellulose - Google Patents
A method of extracting agricultural stalk class waste cellulose Download PDFInfo
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- CN109722932A CN109722932A CN201910128864.4A CN201910128864A CN109722932A CN 109722932 A CN109722932 A CN 109722932A CN 201910128864 A CN201910128864 A CN 201910128864A CN 109722932 A CN109722932 A CN 109722932A
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Abstract
The invention discloses a kind of methods for extracting agricultural stalk class waste cellulose, comprising: agricultural stalk class waste is washed, is dried, crushed into 40 mesh~60 mesh materials；Material is uniformly mixed with high boiling organic solvent-water, under catalyst Lewis Acid metal salt action, is stirred to react at normal pressure, 130~160 DEG C of temperature, and crude fibre is obtained.The method of the present invention utilize recyclable resources agricultural stalk class waste, mild condition, normal pressure, compared under low temperature through the short time processing can efficient selective separate lignocellulosic, realize agricultural stalk class waste cellulose 100% recycle；And the method for the present invention is low to processing unit requirement, it is highly-safe.
Description
Technical field
The invention belongs to farm crop straw organism matter chemical technology fields, are related to a kind of benefit extraction agricultural stalk class waste
It is fine that the method for cellulose more particularly to a kind of utilization high boiling organic solvent and metal salt catalyst extract agricultural stalk class waste
The method for tieing up element.
Background technique
With the propulsion of Tendency of Agricultural Machinery in China, crop planting production method gradually plants transition farm kind by peasant
It plants, adjoint agricultural waste material is also increasing year by year.Agricultural waste material is mainly stalk biomass, as rice straw,
Wheat straw waste, corn stover, cotton stalk, rape stalk, soybean stalk etc..2016, China's agricultural crop straw class waste
Have reached 800,000,000 tons.However, agricultural crop straw class waste is renewable duration biomass resource, the processing side that the country uses
Fado is on-site incineration or production solid molding fuel, also has minority to be used for straw-returning.In short, at present to crops straw
The processing of stalk class waste there are environmental pollution, it is devalued utilize, processing cost is high the defects of, cause the very big wave of resource
Take.
The life of bioenergy and high additive value biobased products is realized in inventor's discovery by lignocellulose-like biomass
Object refining technology is faced with many bottleneck problems, and wherein lignocellulosic-sugar platform lignocellulosic material component separates (i.e.
Wood fiber biomass pretreatment) the problem of it is especially prominent.Studies have shown that lignocellulosic material has complicated chemical group
It is not preprocessed to be difficult to directly by cellulose degraded at the structure with quite densification.Therefore, it is necessary to lignocellulosic material
It carries out component separating treatment and realizes cellulose high efficiente callback, wood fiber biomass enzymatic hydrolysis could be used for.
Currently, lignocellulose raw material components separation method has: diluted acid method, diluted alkaline method and the quick-fried method of steam/ammonia etc..But
These methods are mostly carried out in high-temperature and high-pressure conditions, and the problem of equal various degrees, as cellulose loss is larger, to equipment
Quality requirement height etc., it is difficult to meet the requirement of lignocellulose raw material biorefinery type component separation.In response to this problem, part
High boiling organic solvent gradually draws the concern of domestic and international researcher, such as glycerol by its thermal stability and resolvability (lignin)
With ethylene glycol (L í sias et al., BioresourceTechnol, 2011,102:10040-10046).Grandson pays Poly recruitment
Industry glycerol handles wheat straw as solvent, handles 3h at 220 DEG C of temperature, realizes high-recovery (~98%) (Sun of cellulose
et al.,BioresourceTechnol,2015,187:354–361).Martin C etc. in glycerite by adding
H2SO4As catalyst treatment bagasse, 1h is handled at 190 DEG C of temperature, so that cellulose purity reaches in matrix after processing
72% (Martin et al., Cell ChemTechnol, 2011,45:487-494).Above method is organic molten using higher boiling
Agent processing biomass can effectively avoid the loss of cellulose, but need to handle the long period at high temperature, increase and be processed into
This.
Summary of the invention
The purpose of the present invention is require high, processing for existing lignocellulose raw material components separation method treatment conditions
Problem at high cost is provided a kind of method for extracting agricultural stalk class waste cellulose, is made using high boiling organic solvent-water
For reaction medium, and using Lewis Acid metal salt as catalyst, and treatment conditions are regulated and controled, selectively extracts agricultural
Cellulose in stalk waste.
The purpose of the present invention is what is be achieved through the following technical solutions:
A method of extracting agricultural stalk class waste cellulose, comprising: agricultural stalk class waste is washed, dry
It is dry, it is ground into 40 mesh~60 mesh materials；Material is uniformly mixed with high boiling organic solvent-water, under the action of catalyst at heating
Reason obtains crude fibre.
The agricultural stalk class waste be rice straw, wheat straw waste, corn stover, cotton stalk, rape stalk,
One or more of soybean stalk.
The agricultural stalk class waste is dry to water content 10%~15%.
The agricultural stalk class waste avoids the structure change of cellulose using being mechanically pulverized to 40 mesh~60 mesh
If crystallinity reduces, to guarantee the complete recycling of cellulose.
In addition to considering that high boiling organic solvent is outside one's consideration to lignin dissolution, it is also necessary to be influenced when avoiding the ratio of water excessive anti-
The boiling point of system is answered to change the temperature for leading to not reach heat treatment.Therefore, the high boiling organic solvent and water are controlled
Volume ratio (v/v) be 60:40~95:5.The high boiling organic solvent is one of glycerol and ethylene glycol.
The catalyst is Lewis Acid metal salt；The Lewis Acid metal salt is FeCl3、Fe2(SO4)3、
AlCl3、CuCl2And CuSO4One or more of, preferably FeCl3、AlCl3。
Concentration of the catalyst in high boiling organic solvent-water be 0.015~0.2mol/L, preferably 0.03~
0.12mol/L.Specifically, the catalyst is AlCl3、FeCl3When, concentration of the catalyst in high boiling organic solvent-water
For 0.015~0.1mol/L, preferably 0.03~0.06mol/L.The catalyst is Fe2(SO4)3、CuCl2Or CuSO4When,
Concentration of the catalyst in high boiling organic solvent-water is 0.1~0.12mol/L.
The amount ratio of the agricultural stalk class waste and catalyst is 1g:0.0003~0.004mol, preferably 1g:
0.0006~0.0024mol.
The heat treatment is to be stirred to react 0.2~1h at normal pressure, 130~160 DEG C of temperature.
Preferably, the heat treatment is under normal pressure, while stirring with the heating rate of 12~16 DEG C/min by room
Temperature rise keeps the temperature 0.2~1h to 130~160 DEG C, then is cooled to 50 DEG C or so with the rate of temperature fall of 5~10 DEG C/min.
Specifically, the method for the described extraction agricultural stalk class waste cellulose the following steps are included:
Step (1), agricultural stalk class waste wash de- sandy soil, and natural air drying is crushed to water content 10%~15%
The short thin shape material of 40 mesh~60 mesh；
The material that step (1) obtains is uniformly mixed by step (2) with high boiling organic solvent-water, and catalyst is added, adds
Solid is obtained by filtration in heat treatment, and washing is to neutrality to get crude fibre.
Crude fibre made from the method for the present invention can be further hydrolyzed to through cellulase fermentable sugar (glucose and
Xylose), the production for bio-fuels such as biodiesel, microbial oil, cellulosic ethanol, butanediols.
Beneficial effects of the present invention:
1, the present invention is renewable duration resource using agricultural stalk class waste as raw material；
2, using high boiling organic solvent and water as reaction medium, water is used for catalyst-solvent, makes higher boiling the present invention
Organic solvent-water-catalyst is at homogeneous；In addition, in wood fibre structure, hemicellulose is primarily present in cellulose and wooden
Plain intermediate, Lewis Acid metal salt is dissolved in after water in acidity, generates hydrogen ion (H3O+), it is catalyzed hydrogen bond in lignocellulosic
It is disconnected with part ion key, but is unlikely to decomposition of cellulose, so that a large amount of lignin and hemicellulose are selectively removed, half
Cellulose degradation product monosaccharide, furfural, acetic acid and formic acid etc. are soluble in water, and lignin dissolution is fine in high boiling organic solvent
Dimension element retains；In particular during a heating process, high boiling organic solvent is not easy loss, it can be achieved that recycling.
3, the method for the present invention mild condition, being capable of efficient selective separation wood through short time processing under normal pressure, low temperature
Matter cellulose, the rate of recovery of cellulose is 90~100% in agricultural stalk class waste, hemicellulose removal efficiency is 80%~
95%, delignification rate is 80%~90%.The content of cellulose is 50%~80% in crude fibre obtained, hemicellulose
Cellulose content is 3%~15%, and content of lignin is 5%~12%.The specific surface area of crude fibre is 5~15m2/ g, pore capacities
For 0.01~0.035cm3/ g, aperture are 1.6~2nm.
4, the method for the present invention requires processing unit low, highly-safe.
Detailed description of the invention
Fig. 1 is the electron microscope scanning picture of original rice straw.
Fig. 2 is the electron microscope scanning picture of 4 crude fibre of embodiment.
Specific embodiment
It is right combined with specific embodiments below in order to make those skilled in the art better understand technical solution of the present invention
The present invention is further described.Those skilled in the art can be suitably modified realization of process parameters under the teachings of the present invention.
In particular, it should be pointed out that all similar substitutions and modifications are apparent to those skilled in the art, Ta Mendou
It is deemed to be included in the present invention.
Embodiment 1
Rice straw (containing 34% cellulose, 20% hemicellulose and 26% lignin) washs de- sandy soil, natural air drying
To water content 10%, it is crushed to the short thin shape material of 40 mesh~60 mesh.The smashed rice of 5g is packed into three hole flasks (500mL)
Stalk, 100mL Glycol Mixture (v/v, 90:10) and Aluminum Chloride Hexahydrate, Aluminum Chloride Hexahydrate is in Glycol Mixture
Concentration is 0.006mol/L, is placed in intelligent temperature control digital display heating mantle (ZNHW-500mL, Shanghai Yue Zhong Instrument and Equipment Company), whole
Guarantee to be uniformly mixed by mechanical stirring (150rpm).By being inserted into subsurface thermocouple monitoring temperature, 8-10min is interior by room
Warm (25 DEG C -30 DEG C) rise to 150 DEG C, keep the temperature 30min；Heating mantle is removed, 50 DEG C or so are cooled in 15-20min, takes out three
Hole flask, using sand core funnel (G1-100mL), vacuum filtration obtains solid；Solid is washed with deionized 3 times (every time
200mL deionized water) to filtrate neutrality, obtain crude fibre.
Embodiment 2
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and Aluminum Chloride Hexahydrate, concentration of the Aluminum Chloride Hexahydrate in Glycol Mixture are 0.017mol/L, are placed in
Intelligent temperature control digital display heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm).By being inserted into subsurface thermoelectricity
Even monitoring temperature, 8-10min is interior to rise to 150 DEG C by room temperature (25 DEG C -30 DEG C), keeps the temperature 30min；Heating mantle is removed, in 15-
It is cooled to 50 DEG C or so in 20min, takes out three hole flasks, using sand core funnel, vacuum filtration obtains solid；Solid deionization
Water washing obtains crude fibre to filtrate neutrality.
Embodiment 3
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and Aluminum Chloride Hexahydrate, concentration of the Aluminum Chloride Hexahydrate in Glycol Mixture are 0.039mol/L, are placed in
Intelligent temperature control digital display heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm).By being inserted into subsurface thermoelectricity
Even monitoring temperature, 8-10min is interior to rise to 150 DEG C by room temperature (25 DEG C -30 DEG C), keeps the temperature 30min；Heating mantle is removed, in 15-
It is cooled to 50 DEG C or so in 20min, takes out three hole flasks, using sand core funnel, vacuum filtration obtains solid；Solid deionization
Water washing obtains crude fibre to filtrate neutrality.
Embodiment 4
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and Aluminum Chloride Hexahydrate, concentration of the Aluminum Chloride Hexahydrate in Glycol Mixture are 0.055mol/L, are placed in
Intelligent temperature control digital display heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm).By being inserted into subsurface thermoelectricity
Even monitoring temperature, 8-10min is interior to rise to 150 DEG C by room temperature (25 DEG C -30 DEG C), keeps the temperature 30min；Heating mantle is removed, in 15-
It is cooled to 50 DEG C or so in 20min, takes out three hole flasks, using sand core funnel, vacuum filtration obtains solid；Solid deionization
Water washing obtains crude fibre to filtrate neutrality.The result shows that content of cellulose reaches 76% in crude fibre, hemicellulose and
Content of lignin is down to 4% and 7% respectively, i.e., cellulose removes 90% hemicellulose by 100% recycling respectively in rice straw
With 88% lignin.
After ethylene glycol-aluminium chloride processing, rice straw is originally fine and close, smooth surface (such as Fig. 1) is broken, and shows as
Loose structure (such as Fig. 2).In addition, the crystallinity of crude fibre is 64.2%, specific surface area, pore capacities and aperture are respectively reached
9.8m2/ g, 26.3 × 10-3cm3/ g and 1.9nm.
Embodiment 5
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and Aluminum Chloride Hexahydrate, concentration of the Aluminum Chloride Hexahydrate in Glycol Mixture are 0.083mol/L, are placed in
Intelligent temperature control digital display heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm).By being inserted into subsurface thermoelectricity
Even monitoring temperature, 8-10min is interior to rise to 150 DEG C by room temperature (25 DEG C -30 DEG C), keeps the temperature 30min；Heating mantle is removed, in 15-
It is cooled to 50 DEG C or so in 20min, takes out three hole flasks, using sand core funnel, vacuum filtration obtains solid；Solid deionization
Water washing obtains crude fibre to filtrate neutrality.
Embodiment 6
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and FeCl3, FeCl3Concentration in Glycol Mixture is 0.06mol/L, is placed in intelligent temperature control digital display
Heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm), rise to 150 by room temperature (25 DEG C -30 DEG C) in 8-10min
DEG C, keep the temperature 30min；Heating mantle is removed, is cooled to 50 DEG C or so in 15-20min, takes out three hole flasks, using sand core funnel,
Vacuum filtration obtains solid；Filtrate neutrality is washed with deionized in solid, obtains crude fibre.
Embodiment 7
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and 0.1mol/L Fe2(SO4)3, Fe2(SO4)3Concentration in Glycol Mixture is 0.1mol/L, is set
In intelligent temperature control digital display heating mantle, whole process guarantees to be uniformly mixed by mechanical stirring (150rpm), by room temperature (25 in 8-10min
DEG C -30 DEG C) 150 DEG C are risen to, keep the temperature 30min；Heating mantle is removed, 50 DEG C or so are cooled in 15-20min, three holes is taken out and burns
Bottle, using sand core funnel, vacuum filtration obtains solid；Solid deionized water obtains crude fibre to filtrate neutrality.
Embodiment 8
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) and 0.1mol/L CuSO4, CuSO4Concentration in Glycol Mixture is 0.1mol/L, is placed in intelligence
Temperature control digital display heating mantle, whole process guarantee to be uniformly mixed by mechanical stirring (150rpm), by (25 DEG C -30 of room temperature in 8-10min
DEG C) 150 DEG C are risen to, keep the temperature 30min；Heating mantle is removed, 50 DEG C or so are cooled in 15-20min, takes out three hole flasks, benefit
With sand core funnel, vacuum filtration obtains solid；Solid is washed with deionized to filtrate neutrality, obtains crude fibre.
Comparative example 1
The smashed rice straw of 5g (with embodiment 1), 100mL ethylene glycol-water-soluble are packed into three hole flasks (500mL)
Liquid (v/v, 90:10) is placed in intelligent temperature control digital display heating mantle, and whole process guarantees to be uniformly mixed by mechanical stirring (150rpm), 8-
150 DEG C are risen to by room temperature (25 DEG C -30 DEG C) in 10min, keeps the temperature 30min；Heating mantle is removed, 50 DEG C are cooled in 15-20min
Three hole flasks are taken out in left and right, and using sand core funnel, vacuum filtration obtains solid；Solid is washed with deionized to filtrate neutrality,
Obtain crude fibre.
Table 1: the treatment effect of different catalysts
Claims (10)
1. a kind of method for extracting agricultural stalk class waste cellulose, characterized by comprising: agricultural stalk class waste warp
It washs, be dried, crushed into 40 mesh~60 mesh materials；Material is uniformly mixed with high boiling organic solvent-water, under the action of catalyst
Heat treatment obtains crude fibre.
2. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that the agriculture
Industry stalk waste is one of rice straw, wheat straw waste, corn stover, cotton stalk, rape stalk, soybean stalk
Or it is several.
3. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that the height
The volume ratio of high boiling organic solvent and water is 60:40~95:5 in boiling point organic solvent-water.
4. the method according to claim 1 or 3 for extracting agricultural stalk class waste cellulose, it is characterised in that described
High boiling organic solvent is one of glycerol and ethylene glycol.
5. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that described urges
Agent is Lewis Acid metal salt.
6. the method according to claim 5 for extracting agricultural stalk class waste cellulose, it is characterised in that described urges
Agent is FeCl3、Fe2(SO4)3、AlCl3、CuCl2And CuSO4One or more of.
7. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that described urges
Concentration of the agent in high boiling organic solvent-water is 0.015~0.2mol/L, preferably 0.03~0.12mol/L.
8. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that the agriculture
The amount ratio of industry stalk waste and catalyst be 1g:0.0003~0.004mol, preferably 1g:0.0006~
0.0024mol。
9. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that described adds
Heat treatment is to be stirred to react 0.2~1h at normal pressure, 130~160 DEG C of temperature.
10. the method according to claim 1 for extracting agricultural stalk class waste cellulose, it is characterised in that including as follows
Step:
Step (1), the washing of agricultural stalk class waste, dry, pulverize to 40 mesh~60 mesh materials；
The material that step (1) obtains is uniformly mixed by step (2) with high boiling organic solvent-water, addition catalyst, at heating
Solid is obtained by filtration in reason, and washing is to neutrality to get crude fibre.
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Cited By (5)
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| CN114197233A (en) * | 2021-12-17 | 2022-03-18 | 大连理工大学 | Method for separating and extracting cellulose nanofibers from agricultural and forestry solid wastes |
| CN114717278A (en) * | 2021-01-06 | 2022-07-08 | 江南大学 | Agricultural and forestry biomass pretreatment method |
| CN115196998A (en) * | 2022-07-19 | 2022-10-18 | 东华大学 | Method for enhancing hydrothermal humification of cellulose waste biomass |
| CN115785035A (en) * | 2023-02-03 | 2023-03-14 | 中国农业科学院农业环境与可持续发展研究所 | Method for preparing furfural and 5-hydroxymethylfurfural from straws |
| CN115928479A (en) * | 2022-11-17 | 2023-04-07 | 安徽工程大学 | Method for efficiently deconstructing lignocellulose raw material by coupling carbon dioxide with organic solvent |
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