CN109880865A - A kind of high-efficiency separation and transformation method of corn stover - Google Patents
A kind of high-efficiency separation and transformation method of corn stover Download PDFInfo
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- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 42
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 42
- 235000005822 corn Nutrition 0.000 title claims abstract description 42
- 239000010907 stover Substances 0.000 title claims abstract description 31
- 238000011426 transformation method Methods 0.000 title claims abstract 3
- 240000008042 Zea mays Species 0.000 title abstract description 40
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- 238000006243 chemical reaction Methods 0.000 claims description 41
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000007974 sodium acetate buffer Substances 0.000 claims description 18
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 17
- 108010059892 Cellulase Proteins 0.000 claims description 14
- 229940106157 cellulase Drugs 0.000 claims description 14
- 239000011780 sodium chloride Substances 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 8
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 7
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 7
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 7
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims 3
- 241000209149 Zea Species 0.000 claims 2
- 230000002255 enzymatic effect Effects 0.000 claims 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims 2
- 238000002955 isolation Methods 0.000 claims 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
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- 229940088598 enzyme Drugs 0.000 description 16
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- 239000011734 sodium Substances 0.000 description 6
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 5
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 239000002841 Lewis acid Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
本发明的目的在于提供一种玉米秸秆的高效分离与转化方法，其包括：(1)半纤维素的分离与转化；(2)纤维素的分离与转化；(3)木质素的分离。本发明提供了一种系统的玉米秸秆的高效分离和转化的方法，有效的利用玉米秸秆作为原料，生产高附加值的能源化学品、材料。其中，玉米秸秆当中的半纤维素被分离转化为糠醛，且糠醛得率较高；纤维素被分离转化为高浓度的葡萄糖液；分离得到的木质素，经过鉴定其结构较完整。本发明可以有效的提高三大组分的分离效率与利用率，对于玉米秸秆生物质资源利用和环境保护具有重要意义。The purpose of the present invention is to provide a high-efficiency separation and transformation method of corn stover, which comprises: (1) separation and transformation of hemicellulose; (2) separation and transformation of cellulose; (3) separation of lignin. The present invention provides a systematic method for efficient separation and transformation of corn stalks, which effectively utilizes the corn stalks as raw materials to produce high value-added energy chemicals and materials. Among them, the hemicellulose in the corn stover was separated and converted into furfural, and the yield of furfural was high; the cellulose was separated and converted into a high-concentration glucose solution; the isolated lignin was identified as having a relatively complete structure. The invention can effectively improve the separation efficiency and utilization rate of the three components, and is of great significance to the utilization of corn stover biomass resources and environmental protection.
Description
Technical field
The invention belongs to the separation of biomass full constituent and trans-utilization field, and in particular to a kind of corn stover is efficiently divided
From with method for transformation.
Background technique
China is corn planting economic development big country, while corn yield increasing, the total amount for the corn stover discarded every year
Up to several hundred million tons.Byproduct of the corn stover as grain has many advantages, such as renewable, environmentally friendly, a large amount of supplies, is a kind of great
The petroleum resources substitute of attraction.On the other hand, a large amount of corn stover is not effectively utilized, and does not pass through system
Processing is just directly discharged in the ecosystem, is become agricultural straw refuse, is caused the waste of resource and the dirt of environment
Dye, green, environmental-friendly corn stover cause negative effect to soil, atmosphere, microorganism etc. originally.Therefore, how to have
Effect using corn stover as raw material, produce energy chemistry product, the material of high added value, for environmental protection have important meaning
Justice.
Corn stover is one kind of wood fiber biomass, mainly contains three kinds of cellulose, hemicellulose and lignin groups
Part.In general, the usually hydrolyzed fermentation of cellulose is bio-ethanol, and hemicellulose and lignin can be converted into high add
The chemicals and product of value, such as furfural.Currently, the existing technology to corn stover separation conversion, is difficult to realize to cellulose, half
Cellulose and the big component of lignin three carry out efficient separation and conversion.Wherein, to be produced using hemicellulose in corn stover
Industrial process based on furfural, it is most of be use strong inorganic acid to carry out in the single_phase system of water as catalyst, such as
Sulfuric acid or hydrochloric acid.However using inorganic acid as catalyst, there is shortcomings, lead to difficulty as cellulose decomposition degree is higher
It is significant etc. to carry out later use, inorganic acid severe corrosion to equipment, safety problem.Meanwhile in the single_phase system of water, furfural
Once being formed, it is particularly easy to degrade by resinification reaction and condensation reaction, catabolite is that the insoluble by-product corruption of black is planted
Matter seriously affects furfural yield.Diphasic system is constituted using organic solvent and sodium chloride solution, biomass material is located in advance
Reason, can effectively improve furfural yield, principle is after furfural is formed, by into organic phase, making to degrade furfural extraction
Reaction is preferably minimized, and avoids subsequent adverse effect.Corn stover is in the two-phase formed by organic solvent and sodium chloride solution
After system processing, the organic phase rich in furfural be easy to it is separated from the water open, allow the water phase rich in catalyst to carry out weight
It is multiple to utilize, rich cellulose-containing solid residue is left for further fermenting.
The purpose of the present invention is developing a kind of method for efficiently separating and converting of the corn stover of system, to obtain compared with
The lignin of high furfural yield and enzymolysis efficiency and structural integrity, reaches cellulose in corn stover, hemicellulose, wood
The big component of quality three efficiently separating and converting.
Summary of the invention
The purpose of the present invention is to provide a kind of corn stover efficiently separate and method for transformation.This method is easy to operate,
While obtaining furfural using the hemicellulose in corn stover, the cellulose in the first solid is largely retained in rear
There is higher enzymolysis efficiency in the first continuous enzymolysis process, and still stays in the lignin knot in the second solid after enzymatic hydrolysis
Structure is relatively complete.
The object of the invention to solve the technical problems adopts the following technical solutions to realize:
1, a kind of corn stover proposed according to the present invention efficiently separate and method for transformation, comprising the following steps:
The separation and conversion of hemicellulose: being broken to 20-80 mesh for corn stalk powder, with organic solvent and sodium chloride solution institute
The diphasic system of composition is blended, and catalyst is added, and is rapidly heated and is carried out the first reaction to the first temperature, after reaction,
First is carried out first to be separated by solid-liquid separation, and obtains the first solid and the first liquid, organic phase and water phase then are carried out to the first liquid
Separation, obtains the first organic phase and the first water phase, wherein hemicellulose is converted into furfural and is present in the first organic phase, rich
The first water phase containing catalyst may be repeated utilization；
The separation and conversion of cellulose: the first solid of gained being placed in acetic acid-sodium acetate buffer solution and carries out the first dipping,
Then cellulase is added, carries out the first enzymatic hydrolysis, then carries out second and is separated by solid-liquid separation, obtain the second solid and second liquid,
Middle cellulose is converted into glucose and is present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
The object of the invention to solve the technical problems also can be used following technical measures and further realize:
Preferably, preparation method above-mentioned, wherein hemicellulose separation is 160-180 DEG C with conversion temperature, it is described
Reaction time is 30-60 minutes, and the catalyst concn is 0.05-0.50mol/L.
Preferably, preparation method above-mentioned, wherein the acetic acid-sodium acetate buffer solution concentration is 50mmol/L, pH is
4.7-4.9；Used dip time is 12-24 hours；The solid-to-liquid ratio of used solid residue and sodium acetate solution is 1:20-
50g/mL；The enzyme activity of used cellulase is to contain 15-20 filter paper enzyme activity unit in every gram of substrate；The enzymolysis time is
36-72 hours, temperature was 50-55 DEG C.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize:
A kind of corn stover proposed according to the present invention efficiently separate and method for transformation, the corn stover it is efficient
Separation can be realized with conversion by method described in any of the above embodiments.
By above-mentioned technical proposal, the efficiently separating with method for transformation of corn stover of the invention at least has following excellent
Point:
(1) compared with traditional acid catalyst dehydration prepares furfural, using there is bronsted acid and lewis acid simultaneously
Property metal nitrate as catalyst, the destruction journey to cellulose and lignin can be reduced while improving furfural yield
Degree.
(2) compared with the pretreatment of the single_phase system of traditional water, the diphasic system of organic solvent and water can be in furfural in water
It while formation in phase, is extracted into the first organic phase, is effectively reduced the resinification reaction and condensation reaction of furfural,
The a large amount of generations for avoiding humus, effectively raise the yield of furfural.
(3) it is compared with the traditional method, hemicellulose, which is converted into the solid waste after furfural, can obtain height by enzymatic hydrolysis
The Glucose Liquid of concentration realizes the effective use to cellulose, and is still largely retained in the second solid after enzymatic hydrolysis
Lignin, structure retain it is more complete.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, with presently preferred embodiments of the present invention, detailed description is as follows below.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to a kind of its specific embodiment of the method for comprehensive utilization of corn stover proposed according to the present invention, feature and
Its performance, detailed description is as follows.In the following description, what different " embodiment " or " embodiment " referred to is not necessarily same reality
Apply example.In addition, the special characteristic, structure or feature in one or more embodiments can be combined by any suitable form.
The embodiment of the present invention propose a kind of corn stover efficiently separate and method for transformation.
The preparation method the following steps are included:
The separation and conversion of hemicellulose: being broken to 20-80 mesh for corn stalk powder, methyl iso-butyl ketone (MIBK) or tetrahydrofuran and
Concentration is ratio composition diphasic system of the 10-30wt% sodium chloride solution according to 1:0.5-2.0, by corn stover and diphasic system
It is blended, the metal nitrate that 0.01-1.00mol/L is added makees catalyst, and being rapidly heated to 120-200 DEG C, it is anti-to carry out first
It answers, reaction temperature is 120-200 DEG C, and the reaction time is 15-150 minutes.After reaction, first is carried out first to be separated by solid-liquid separation,
Obtain the first solid and the first liquid, then to the first liquid carry out organic phase and water phase separation, obtain the first organic phase with
First water phase, wherein hemicellulose is converted into furfural and is present in the first organic phase, and the first water phase rich in catalyst can be with
It is reused；
The separation and conversion of cellulose: it is 50mmol/L that the first solid of gained, which is placed in concentration, and pH is the second of 4.6-5.0
12-24 hours the first dippings, the solid-to-liquid ratio of the first solid and acetic acid-sodium acetate buffer solution are carried out in acid-sodium acetate buffer
For 1:20-50g/mL, cellulase is then added, the enzyme activity of cellulase is to contain 10-20 filter paper enzyme activity in every gram of substrate
Unit, carries out the enzymatic hydrolysis of 3-72 hour first in 40-60 DEG C of environment, then carries out second and is separated by solid-liquid separation, obtains the second solid
And second liquid, wherein cellulose is converted into glucose and is present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
With specific embodiment, the present invention will be further described below, but not as the limitation of the invention.
Embodiment 1
The separation and conversion of hemicellulose: corn stalk powder is broken to 20-80 mesh, methyl iso-butyl ketone (MIBK) and concentration are
20wt% sodium chloride solution forms diphasic system according to the ratio of 1:1, and corn stover is blended with diphasic system, is added
The chromic nitrate of 0.05mol/L is rapidly heated as catalyst and carries out the first reaction to 160 DEG C, and reaction temperature is 160 DEG C, reaction
Time is 30 minutes.After reaction, first is carried out first to be separated by solid-liquid separation, the first solid and the first liquid are obtained, then to the
One liquid carries out the separation of organic phase and water phase, obtains the first organic phase and the first water phase, wherein hemicellulose is converted into furfural
It is present in the first organic phase, the first water phase rich in catalyst may be repeated utilization；
The separation and conversion of cellulose: it is 50mmol/L, acetic acid-second that pH is 4.7 that the first solid of gained, which is placed in concentration,
12 hours the first dippings are carried out in sour sodium buffer, the solid-to-liquid ratio of the first solid and acetic acid-sodium acetate buffer solution is 1:50g/
Then cellulase is added in mL, the enzyme activity of cellulase is to contain 20 filter paper enzyme activity units in every gram of substrate, in 50 DEG C of ring
It carries out 60 hours first digesting in border, then carries out second and be separated by solid-liquid separation, obtain the second solid and second liquid, wherein cellulose
Glucose is converted into be present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
The furfural and Glucose Liquid obtained using the present embodiment carries out Concentration Testing, and obtaining its furfural yield is 34.2%, enzyme
Solving saccharification efficiency is 84.9%, and the solid residue to gained rich in lignin carries out Structural Identification, as the result is shown the knot of lignin
Structure retains more complete.
Embodiment 2
The separation and conversion of hemicellulose: corn stalk powder is broken to 20-80 mesh, methyl iso-butyl ketone (MIBK) and concentration are
10wt% sodium chloride solution forms diphasic system according to the ratio of 1:0.5, and corn stover is blended with diphasic system, is added
The aluminum nitrate of 0.10mol/L is rapidly heated as catalyst and carries out the first reaction to 160 DEG C, and reaction temperature is 160 DEG C, reaction
Time is 60 minutes.After reaction, first is carried out first to be separated by solid-liquid separation, the first solid and the first liquid are obtained, then to the
One liquid carries out the separation of organic phase and water phase, obtains the first organic phase and the first water phase, wherein hemicellulose is converted into furfural
It is present in the first organic phase, the first water phase rich in catalyst may be repeated utilization；
The separation and conversion of cellulose: it is 50mmol/L, acetic acid-second that pH is 4.8 that the first solid of gained, which is placed in concentration,
24 hours the first dippings are carried out in sour sodium buffer, the solid-to-liquid ratio of the first solid and acetic acid-sodium acetate buffer solution is 1:50g/
Then cellulase is added in mL, the enzyme activity of cellulase is to contain 15 filter paper enzyme activity units in every gram of substrate, in 55 DEG C of ring
It carries out 36 hours first digesting in border, then carries out second and be separated by solid-liquid separation, obtain the second solid and second liquid, wherein cellulose
Glucose is converted into be present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
The furfural and Glucose Liquid obtained using the present embodiment carries out Concentration Testing, and obtaining its furfural yield is 48.0%, enzyme
Solving saccharification efficiency is 85.5%, and the solid residue to gained rich in lignin carries out Structural Identification, and fruit shows the structure of lignin
Retain more complete.
Embodiment 3
The separation and conversion of hemicellulose: corn stalk powder is broken to 20-80 mesh, tetrahydrofuran and concentration are 30wt% chlorine
Change sodium solution and form diphasic system according to the ratio of 1:1, corn stover is blended with diphasic system, 0.50mol/L is added
Aluminum nitrate as catalyst, be rapidly heated to 160 DEG C carry out first reaction, reaction temperature be 160 DEG C, the reaction time be 60 points
Clock.After reaction, first is carried out first to be separated by solid-liquid separation, obtain the first solid and the first liquid, then the first liquid is carried out
The separation of organic phase and water phase obtains the first organic phase and the first water phase, wherein hemicellulose is converted into furfural and is present in first
In organic phase, the first water phase rich in catalyst may be repeated utilization；
The separation and conversion of cellulose: it is 50mmol/L, acetic acid-second that pH is 4.9 that the first solid of gained, which is placed in concentration,
12 hours the first dippings are carried out in sour sodium buffer, the solid-to-liquid ratio of the first solid and acetic acid-sodium acetate buffer solution is 1:20g/
Then cellulase is added in mL, the enzyme activity of cellulase is to contain 15 filter paper enzyme activity units in every gram of substrate, in 55 DEG C of ring
It carries out 72 hours first digesting in border, then carries out second and be separated by solid-liquid separation, obtain the second solid and second liquid, wherein cellulose
Glucose is converted into be present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
The furfural and Glucose Liquid obtained using the present embodiment carries out Concentration Testing, and obtaining its furfural yield is 25.0%, enzyme
Solving saccharification efficiency is 44.6%, and the solid residue to gained rich in lignin carries out Structural Identification, and fruit shows the structure of lignin
Retain more complete.
Embodiment 4
The separation and conversion of hemicellulose: corn stalk powder is broken to 20-80 mesh, tetrahydrofuran and concentration are 10wt% chlorine
Change sodium solution and form diphasic system according to the ratio of 1:0.5, corn stover is blended with diphasic system, 0.10mol/ is added
The chromic nitrate of L is rapidly heated as catalyst and carries out the first reaction to 180 DEG C, and reaction temperature is 180 DEG C, the reaction time 30
Minute.After reaction, first carry out first be separated by solid-liquid separation, obtain the first solid and the first liquid, then to the first liquid into
The separation of row organic phase and water phase obtains the first organic phase and the first water phase, wherein hemicellulose is converted into furfural and is present in
In one organic phase, the first water phase rich in catalyst may be repeated utilization；
The separation and conversion of cellulose: it is 50mmol/L, acetic acid-second that pH is 4.8 that the first solid of gained, which is placed in concentration,
24 hours the first dippings are carried out in sour sodium buffer, the solid-to-liquid ratio of the first solid and acetic acid-sodium acetate buffer solution is 1:50g/
Then cellulase is added in mL, the enzyme activity of cellulase is to contain 20 filter paper enzyme activity units in every gram of substrate, in 50 DEG C of ring
It carries out 60 hours first digesting in border, then carries out second and be separated by solid-liquid separation, obtain the second solid and second liquid, wherein cellulose
Glucose is converted into be present in second liquid；
The separation of lignin: sufficiently cleaning the second solid using acetic acid-sodium acetate buffer solution, be then dried,
In, lignin is present in solid form in the second solid.
The furfural and Glucose Liquid obtained using the present embodiment carries out Concentration Testing, and obtaining its furfural yield is 42.0%, enzyme
Solving saccharification efficiency is 80.9%, and the solid residue to gained rich in lignin carries out Structural Identification, and fruit shows the structure of lignin
Retain more complete.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (5)
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| CN112876356A (en) * | 2021-01-21 | 2021-06-01 | 青岛科技大学 | Method for converting corn straw into ethyl levulinate and extracting lignin based on two-phase solvent system |
| 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 |
| CN114085252A (en) * | 2021-10-21 | 2022-02-25 | 中国林业科学研究院林产化学工业研究所 | A comprehensive utilization method of organic acid-catalyzed two-phase system for separating wood fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112876356A (en) * | 2021-01-21 | 2021-06-01 | 青岛科技大学 | Method for converting corn straw into ethyl levulinate and extracting lignin based on two-phase solvent system |
| CN112876356B (en) * | 2021-01-21 | 2022-07-05 | 青岛科技大学 | A method for converting corn stover into ethyl levulinate and extracting lignin based on dual-phase solvent system |
| 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 |
| CN114085252A (en) * | 2021-10-21 | 2022-02-25 | 中国林业科学研究院林产化学工业研究所 | A comprehensive utilization method of organic acid-catalyzed two-phase system for separating wood fiber |
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