CN109354635A - A kind of method of hemicellulose in the low co-melting compound alkalinity extraction biomass of solvent - Google Patents
A kind of method of hemicellulose in the low co-melting compound alkalinity extraction biomass of solvent Download PDFInfo
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- CN109354635A CN109354635A CN201811192290.9A CN201811192290A CN109354635A CN 109354635 A CN109354635 A CN 109354635A CN 201811192290 A CN201811192290 A CN 201811192290A CN 109354635 A CN109354635 A CN 109354635A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The present invention provides a kind of methods of hemicellulose in low co-melting compound alkalinity extraction biomass of solvent, the described method comprises the following steps, (1) crushes biomass, drying；(2) low co-melting solvent is prepared using choline chloride and organic acid；(3) low co-melting solvent and powdered biomass are mixed, stirring；(4) mixing liquid after fully reacting is filtered, filter residue and filtrate is separately stored spare；(5) ionized water is added into filtrate and is centrifuged 20min after standing a period of time at 4200rpm, gained sedimentation substance dries to constant weight at 105 DEG C, and natural cooling obtains rugose wood element；(6) filter residue is adopted and is washed with deionized to neutrality, with lye extraction, filtering, it is adjusted to neutrality, it is added after ethyl alcohol stands a period of time and is centrifuged, gained sedimentation substance dries to constant weight at 105 DEG C, and natural cooling obtains hemicellulose, and the present invention is low, and co-melting alkali extraction lignin yield is 7-42 percentage points higher than the prior art, the hemilignin rate of recovery is more than or equal to 78%, and purity is more than or equal to 85%.
Description
Technical field
The present invention relates to technical field of biochemical industry, and in particular in the low co-melting compound alkalinity extraction biomass of solvent of one kind
The method of hemicellulose.
Background technique
Hemilignin is and the close-connected a kind of non-cellulose copolymerization of cellulose, especially lignin is sugared.Hemilignin
Chemical structure is complicated, not only has main chain different in size, there are also the different side chain of structure and various conformations.In addition, half is wooden
Element composition glycosyl it is varied, not only include pentose such as xylose, arabinose, but also including hexose for example rhamnose, galactolipin,
Mannose and glucose etc..The complexity of structure and the diversity of composition, make hemilignin have a wide range of applications in various fields.
In the food industry, hemilignin can be used as food adhesive, thickener, stabilizer and water-setting agent；It is wooden in pharmaceuticals industry, half
Element can be used as sedative, and cholesterol inhibitor, modified xylan can be with anticoagulation；In paper industry, xylan is still
Anti-tear tensile strength can be enhanced in good additive.
The extracting method of hemilignin generally can be divided into direct method and indirect method, and direct method is to utilize lye or organic solvent
Directly biomass is extracted, hemilignin is dissolved out, but the method energy consumption is high and waste water is more, difficult, the half of extraction
Lignin usually contains certain lignin.Indirect method is first to dispose lignin, obtains full lignin and recycles not Tongfang
The extraction of method progress hemilignin.Wheat stalk first is handled with sodium chlorite in CN105111332A patent, destroys lignin knot
Structure promotes the quality of hemilignin, and the extraction of hemilignin is finally carried out using alkaline process.But sodium chlorite is during the reaction
Meeting release chlorine, it is all harmful to human body, environment, and lignin is destroyed, reduce the economic benefit of biomass economy.
CN102603927A patent is then to extract hemilignin using high boiling alcohol boiling and ethyl alcohol sedimentation, and salt acid for adjusting pH is recycled to obtain
To lignin, but lignin yield is very low, and highest yield only 10.8%, do not recycle lignin well.
Summary of the invention
In order to solve, existing hemicellulose extraction efficiency is lower, energy consumption is high, product purity is low, hemicellulose Destruction rate
High problem, the method that the present invention proposes hemicellulose in the low co-melting compound alkalinity extraction biomass of solvent of one kind, first removing is wooden
Element simultaneously, then extracts hemilignin, has both avoided lye for the extracting section of lignin, has also protected the basic knot of hemilignin
Structure.Low co-melting alkali extraction lignin yield is 7-42 percentage points higher than the prior art, and the hemilignin rate of recovery is more than or equal to 78%,
Purity is more than or equal to 85%.
In order to solve the above-mentioned technical problem, the present invention is using half fiber in a kind of low co-melting compound alkalinity extraction biomass of solvent
The method for tieing up element, the described method comprises the following steps,
(1) biomass be crushed into 20-100 mesh, then dried；
(2) using choline chloride for hydrogen bond is receptor, organic acid as be uniformly mixed under hydrogen bond donor room temperature prepare it is low total
Melt and dissolved dose；
(3) powdered biomass of the low co-melting solvent of step (2) preparation and step (1) preparation is pressed into low co-melting solvent volume
It is 1g:5ml-1g:10ml mixing with powdered biomass weight ratio, stirring, mixing time is 6-12 hours, mixing temperature 60-
100℃；
(4) mixing liquid after step (3) fully reacting is filtered, filter residue and filtrate is separately stored spare；
(5) ionized water is added into step (4) resulting filtrate and is centrifuged at 4200rpm after standing a period of time
20min, gained sedimentation substance dry to constant weight at 105 DEG C, and natural cooling obtains rugose wood element；
(6) filter residue in step (4) is adopted and is washed with deionized to neutrality, with lye extraction, filtering, gained filtrate is used
Glacial acetic acid is adjusted to neutrality, and is added after ethyl alcohol stands a period of time and is centrifuged 20min in 4200rpm, and gained settles substance at 105 DEG C
It dries to constant weight, natural cooling obtains hemicellulose.
Preferably, the biomass in above-mentioned steps (1) is in agricultural crop straw, herbaceous plant, timber, shell or fruit stone
One kind.
Preferably, drying temperature is 45-60 DEG C in above-mentioned steps (1), drying time 4-6h.
Preferably, the organic acid used in above-mentioned steps (2) for oxalic acid, lactic acid, malic acid, maleic acid, levulic acid or
One of person's glycolic.
Preferably, deionized water and filtrate volume ratio are 1:1 in above-mentioned steps (5).
Preferably, supernatant liquor obtained in above-mentioned steps (5) recycles low co-melting solvent by rotary evaporation.
Preferably, the lye in above-mentioned steps (6) is the sodium hydroxide solution that mass fraction is 1-8%, and extraction time is
10-24h。
Preferably, ethyl alcohol and neutral filtrate volume ratio are 3:1 in above-mentioned steps (6).
The invention has the benefit that
The present invention, which passes through, first removes lignin, then extracts hemilignin, and lignin is avoided to be blended in hemilignin by alkali
Liquid extracts simultaneously, can be improved the yield and purity of hemilignin；The low co-melting solvent prepared in the present invention is known as wooden
Specificity removing and dissolution, will not destroy in the structural of hemilignin and removing and course of dissolution will not generate pernicious gas,
The more environmentally-friendly, safety compared with existing lignin deviates from technology, lignin yield is 7-42 percentage points higher than the prior art, half wood
The quality rate of recovery is more than or equal to 78%, and purity is more than or equal to 85%.The present invention recycles low co-melting solvent by rotary evaporation, real
Existing solvent is reused, and not only reduces production cost, but also being capable of energy-saving and emission-reduction.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with implementation of the invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1
The present invention provides the method for hemicellulose in the low co-melting compound alkalinity extraction biomass of solvent of one kind, including following step
Suddenly,
Poplar bits are first crushed to 20 mesh, are dried at 45 DEG C.It weighs the poplar bits after 10g is crushed and is put into reactor
In, the DES of 50mL oxalic acid and choline chloride preparation is added, is stirred 6 hours at 85 DEG C, product is filtered later, obtains filtrate
And filter residue.The water that 1 times of volume is added in filtrate is stood, and is centrifuged 20 minutes at 4200rpm later, and sedimentation 105 DEG C of drying of substance are arrived
Constant weight obtains rugose wood element, yield 17%；Supernatant rotary evaporation can recycle DES after removing water；Residue washing is into
Property extracted overnight 12 hours with 1% sodium hydroxide of mass fraction again, with middling speed qualitative filter paper filter after, 1% ice vinegar of filtrate
3 times of 95% ethyl alcohol of volume are added later and stand, are centrifuged 20 minutes in 4200rpm, settle 105 DEG C of substance bakings for acid for adjusting pH=7
It is dry, obtain hemilignin, purity 85%, the hemilignin rate of recovery 78%.
Embodiment 2
The present invention provides the method for hemicellulose in the low co-melting compound alkalinity extraction biomass of solvent of one kind, including following step
Suddenly,
Beautiful wooden core is first crushed to 60 mesh, is dried at 45 DEG C.It weighs the corncob after 10g is crushed and is put into reactor
In, the DES of 100mL malic acid and choline chloride preparation is added, is stirred 8 hours at 85 DEG C, product is filtered later, is filtered
Liquid and filter residue.The water that 1 times of volume is added in filtrate is stood, and is centrifuged 20 minutes at 4200rpm later, and 105 DEG C of substance drying are settled
To constant weight, rugose wood element, yield 35% are obtained；Supernatant rotary evaporation can recycle DES after removing water；Residue washing is extremely
Neutrality is extracted 10 hours with 8% sodium hydroxide of mass fraction overnight again, after being filtered with middling speed qualitative filter paper, 1% ice of filtrate
Acetic acid adjusts pH=7, and 3 times of 95% ethyl alcohol of volume are added later and stand, and is centrifuged 20 minutes in 4200rpm, settles 105 DEG C of substance bakings
It is dry, obtain hemilignin, purity 90%, the hemilignin rate of recovery 86%.
Embodiment 3
The present embodiment provides a kind of method of hemicellulose in low co-melting compound alkalinity extraction biomass of solvent, including it is following
Step,
Straw is first crushed to 80 mesh, is dried at 45 DEG C.It weighs the straw after 10g is crushed to be put into reactor, add
The DES for entering 80mL lactic acid and choline chloride preparation, stirs 10 hours at 85 DEG C, later filters product, obtain filtrate and filter
Slag.The water that 1 times of volume is added in filtrate is stood, and is centrifuged 20 minutes at 4200rpm later, is settled 105 DEG C of substance drying and is arrived constant weight,
Rugose wood element, yield 44% are obtained, supernatant rotary evaporation can recycle DES after removing water；Residue washing to it is neutral again
It is extracted overnight 12 hours with 4% sodium hydroxide of mass fraction, after being filtered with middling speed qualitative filter paper, 1% glacial acetic acid tune of filtrate
PH=7 is saved, 3 times of 95% ethyl alcohol of volume are added later and stand, is centrifuged 20 minutes in 4200rpm, 105 DEG C of substance drying is settled, obtains
To hemilignin, purity 92%, the hemilignin rate of recovery 88%.
Embodiment 4
The present embodiment provides a kind of method of hemicellulose in low co-melting compound alkalinity extraction biomass of solvent, including it is following
Step,
Walnut shell powder is first broken to 100 mesh, is dried at 45 DEG C.It weighs the walnut shell after 50g is crushed and is put into reactor
In, the DES of 250mL lactic acid and choline chloride preparation is added, is stirred 8 hours at 85 DEG C, product is filtered later, obtains filtrate
And filter residue.The water that 1 times of volume is added in filtrate is stood, and is centrifuged 20 minutes at 4200rpm later, 105 DEG C of the substance being centrifuged out bakings
Constant weight is done, rugose wood element, yield 40% are obtained；Supernatant rotary evaporation can recycle DES after removing water；Residue washing
It is extracted overnight 8 hours with 6% sodium hydroxide of mass fraction again to neutrality, after being filtered with middling speed qualitative filter paper, filtrate is with 1%
Glacial acetic acid adjusts pH=7, and 3 times of 95% ethyl alcohol of volume are added later and stand, and is centrifuged 20 minutes in 4200rpm, settles 105 DEG C of substance
Drying, obtains hemilignin, purity 90%, the hemilignin rate of recovery 85%.
Embodiment 5
The present embodiment provides a kind of method of hemicellulose in low co-melting compound alkalinity extraction biomass of solvent, including it is following
Step,
Willow Strip is first crushed to 50 mesh, is dried at 45 DEG C.It weighs the willow Strip after 30g is crushed and is put into reactor
In, the DES of 300mL lactic acid and choline chloride preparation is added, is stirred 12 hours at 100 DEG C, product is filtered later, is filtered
Liquid and filter residue.The water that 1 times of volume is added in filtrate is stood, and is centrifuged 20 minutes at 4200rpm later, and 105 DEG C of substance drying are settled
To constant weight, rugose wood element, yield 52% are obtained, supernatant rotary evaporation can recycle DES after removing water；Residue washing is extremely
Neutrality is extracted 24 hours with 5% sodium hydroxide of mass fraction overnight again, after being filtered with middling speed qualitative filter paper, 1% ice of filtrate
Acetic acid adjusts pH=7, and 3 times of 95% ethyl alcohol of volume are added later and stand, and is centrifuged 20 minutes in 4200rpm, settles substance 105
DEG C drying, obtain hemilignin, purity 97%, the hemilignin rate of recovery 80%.
The yield of the low co-melting extraction rugose wood element of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Yield (%) | 17 | 35 | 44 | 40 | 52 |
According to table 1, when powdered biomass quality and low co-melting solvent volume ratio are 1g:5ml, rugose wood element
Recovery rate have reached 17%, 10% reached than in the prior art improves 7 percentage points；When powdered biomass matter
When amount and low co-melting solvent volume ratio are 1g:10ml, 1g:4ml, 1g:3ml and 1g:2ml, the recovery rate difference of rugose wood element
Reach 35%, 44%, 40% and 52%, 10% reached than in the prior art respectively improves 25,34,30,42 percentages
Point.Compared with the prior art, low co-melting solvent provided by the invention is significantly improved to the recovery rate of rugose wood element.
The 2 hemilignin rate of recovery of table and purity
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| The rate of recovery (%) | 78 | 86 | 88 | 88 | 80 |
| Purity (%) | 85 | 90 | 92 | 90 | 97 |
It is 1%, 8%, 4%, 6% and 5% sodium hydroxide solution to extraction filter residue, gained that mass fraction, which is respectively adopted,
The hemilignin rate of recovery is respectively 78%, 86%, 88%, 88% and 80%, corresponding purity is 85%, 90%, 92%, 90%
With 97%.The results are shown in Table 2.Wherein, when sodium hydroxide solution mass fraction is 4% and 6%, the recycling of gained hemilignin
Rate highest；When sodium hydroxide solution mass fraction is 4% and 5%, gained hemilignin purity highest.
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that:
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement；And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Spirit and scope.
Claims (8)
1. the method for hemicellulose, feature exist in a kind of low co-melting compound alkalinity extraction biomass of solvent, the method includes
Following steps,
(1) biomass be crushed into 20-100 mesh, then dried；
(2) using choline chloride for hydrogen bond is receptor, organic acid as be uniformly mixed under hydrogen bond donor room temperature prepare it is low co-melting molten
Agent；
(3) powdered biomass of the low co-melting solvent of step (2) preparation and step (1) preparation is pressed into low co-melting solvent volume and life
Material powder weight ratio is 1g:5ml-1g:10ml mixing, and stirring, mixing time is 6-12 hours, mixing temperature 60-100
℃；
(4) mixing liquid after step (3) fully reacting is filtered, filter residue and filtrate is separately stored spare；
(5) ionized water is added into step (4) resulting filtrate and is centrifuged 20min at 4200rpm after standing a period of time, institute
Substance must be settled to dry to constant weight at 105 DEG C, natural cooling obtains rugose wood element；
(6) filter residue in step (4) is adopted and is washed with deionized to neutrality, with lye extraction, filtering, gained filtrate ice vinegar
Acid is adjusted to neutrality, and is added after ethyl alcohol stands a period of time and is centrifuged 20min in 4200rpm, and gained sedimentation substance is dried at 105 DEG C
Constant weight, natural cooling obtain hemicellulose.
2. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, the biomass in the step (1) is one of agricultural crop straw, herbaceous plant, timber, shell or fruit stone.
3. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, drying temperature is 45-60 DEG C in the step (1), drying time 4-6h.
4. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, the organic acid used in the step (2) is in oxalic acid, lactic acid, malic acid, maleic acid, levulic acid or glycolic
One kind.
5. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, deionized water and filtrate volume ratio are 1:1 in the step (5).
6. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, supernatant liquor obtained in the step (5) recycles low co-melting solvent by rotary evaporation.
7. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, the lye in the step (6) is the sodium hydroxide solution that mass fraction is 1-8%, extraction time 10-24h.
8. the method for hemicellulose, feature in the low co-melting compound alkalinity extraction biomass of solvent according to claim 1
It is, ethyl alcohol and neutral filtrate volume ratio are 3:1 in the step (6).
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| CN109706768A (en) * | 2019-03-11 | 2019-05-03 | 贵州华清科维环境能源有限责任公司 | A method of extracting Papermaking fibers from vinasse |
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| CN110527111A (en) * | 2019-09-30 | 2019-12-03 | 北京林业大学 | A method of mild and quick separating lignin |
| CN113480580A (en) * | 2021-06-09 | 2021-10-08 | 华南农业大学 | Method for selectively and efficiently extracting licorice residue flavone and co-producing biomethane |
| CN116554576A (en) * | 2023-05-12 | 2023-08-08 | 山东理工大学 | Composite material based on in-situ lignin regeneration and preparation method and application thereof |
| WO2023184994A1 (en) * | 2022-03-30 | 2023-10-05 | 广东邦普循环科技有限公司 | Preparation method for and use of porous microsphere carbon negative electrode material |
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Cited By (11)
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| CN109706768A (en) * | 2019-03-11 | 2019-05-03 | 贵州华清科维环境能源有限责任公司 | A method of extracting Papermaking fibers from vinasse |
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| CN113480580A (en) * | 2021-06-09 | 2021-10-08 | 华南农业大学 | Method for selectively and efficiently extracting licorice residue flavone and co-producing biomethane |
| WO2023184994A1 (en) * | 2022-03-30 | 2023-10-05 | 广东邦普循环科技有限公司 | Preparation method for and use of porous microsphere carbon negative electrode material |
| GB2621714A (en) * | 2022-03-30 | 2024-02-21 | Guangdong Brunp Recycling Technology Co Ltd | Preparation method for and use of porous microsphere carbon negative electrode material |
| CN116554576A (en) * | 2023-05-12 | 2023-08-08 | 山东理工大学 | Composite material based on in-situ lignin regeneration and preparation method and application thereof |
| CN116554576B (en) * | 2023-05-12 | 2024-04-12 | 山东理工大学 | Composite material based on in-situ lignin regeneration and preparation method and application thereof |
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Application publication date: 20190219 |