CN108660837A - The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material - Google Patents
The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material Download PDFInfo
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- CN108660837A CN108660837A CN201810543585.XA CN201810543585A CN108660837A CN 108660837 A CN108660837 A CN 108660837A CN 201810543585 A CN201810543585 A CN 201810543585A CN 108660837 A CN108660837 A CN 108660837A
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- hemicellulose
- lignin
- cellulose
- plant fiber
- eutectic solvent
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Classifications
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- 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
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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
Abstract
The invention discloses the separation methods of three component of cellulose, hemicellulose and lignin in a plant fiber raw material, pressurization is carried out to plant fiber material by lactic acid/choline chloride eutectic solvent or normal heating boiling is handled, selective dissolved lignin and hemicellulose, the remaining washed acquisition cellulose of insoluble matter；Elutriation is added to go out lignin, washed, isolated lignin the eutectic solvent dissolution fluid containing lignin and hemicellulose；The remaining eutectic solvent aqueous solution containing hemicellulose, hemicellulose is obtained through nanofiltration separation；It can be recycled after the concentrated dehydration of eutectic solvent aqueous solution.Being sufficiently separated for plant fiber material each component can be achieved in the present invention, and it is more than the cellulose that the 79.5%, degree of polymerization is up to 1113 to obtain chemical cellulose content, and lignin of the purity more than 89% and yield are more than 45% hemicellulose.Its energy consumption is low, and gained size performance is excellent, has industrial applications foreground.
Description
Technical field
The invention belongs to biomass resources to comprehensively utilize scope, be related to three component of cellulose, hemicellulose and lignin
Separation technology field, and in particular to the separation side of three component of cellulose, hemicellulose and lignin in a plant fiber raw material
Method realizes efficiently separating for plant fiber material each component by novel green eutectic solvent, for new environmentally protective plant
The big plain separating technology of fibres raw material three.
Background technology
In pulp and paper industry, traditional cellulose separation method, such as sulfate process or soda processes, not only production consume
Can be high, and generate in digestion process containing high pollutional load liquid, immense pressure is caused to environment.And it is common
The foul gas that will produce sulfur-bearing in sulfate pulping paper production seriously affects air generation.Therefore, tradition system is broken through
Bottleneck is starched, searching is environmental-friendly, separation is efficient and operable strong green pulping process can not urgently wait for.
Eutectic solvent is one kind by hydrogen bond receptor (such as quaternary ammonium salt) and hydrogen bond donor (such as amide, carboxylic acid and polyalcohol) group
Two components made of conjunction or three component eutectic mixtures, solidification point are less than the fusing point of each component materials, be it is a kind of can be
Liquid is kept under room temperature.Such as choline chloride (hydrogen bond receptor) and urea (hydrogen bond donor) are mixed and can be obtained eutectic
Solvent prepares simply, and is not required to purify.Eutectic solvent can all keep liquid in large temperature range, have good water
The good characteristics such as dissolubility, incombustibility, biological adaptive, biodegradable all have greater advantage at economical and environmentally friendly aspect.It is low
Congruent melting solvent can crack major part β-O-4 keys, to realize lignin in timber, hemicellulose and fiber at a certain temperature
The separation of element.And itself solubility property is limited, does not have solvability substantially to cellulose, it instead can a large amount of dissolved lignins
And hemicellulose.Chinese patent CN105908550A uses lactic acid and pre-processes eucalyptus with benzyltriethylammoinium chloride eutectic solvent
Wood powder may separate out lignin of the purity 90% or more, but the patent is served only for processing wood powder separation and obtains lignin, not
Realize to the comprehensive utilization of three component of plant fiber material and its operating cost it is higher, cause its industrialization to be restricted.
Invention content
Goal of the invention：Serious pollution etc. for water resource caused by traditional pulping and papermaking process and atmospheric environment lacks
It falls into, the object of the present invention is to provide a kind of environmentally protective, efficient plant fiber material three components separation methods, are a kind of environment
Friendly, low energy consumption pulping and paper-making production technology.
Technical solution：In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is as follows：
The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material, including following step
Suddenly：
1) lactic acid of preparation/choline chloride eutectic solvent is added to the plant fiber material air-dried after crushing, by solid-liquid
Mixture, which is added in compressive reaction kettle or normal-pressure reaction kettle, carries out heating boiling processing, obtains eutectic solvent treated mixing
Object；
2) washed by the eutectic solvent being prepared in step 1) treated mixture after strainer squeezes filtering
Liquid washs to obtain insoluble matter cellulose and the eutectic solvent dissolution fluid containing hemicellulose and lignin；
3) by the eutectic solvent dissolution fluid containing hemicellulose and lignin of gained in step 2) it is concentrated after, water is added
It is middle to regenerate isolated lignin and the eutectic solvent aqueous solution containing hemicellulose；
4) it will be obtained by nanofiltration separation after eutectic solvent aqueous solution thickening of the gained containing hemicellulose in step 3)
To hemicellulose.
In step 1), used lactic acid and choline chloride eutectic solvent molar ratio are 3~15:1.
In step 1), plant fiber material is needlebush, leaf wood, bamboo material or grass raw material, and plant fiber is former
Size after feed powder is broken includes the standing grain of the particle of the mesh of 20 mesh~80, the wood chip of 1~2cm of long 2~4cm wide or bamboo chip, long 2~4cm
Grass as raw material.
In step 1), the solid-to-liquid ratio of used plant fiber material and eutectic solvent is 1:3~1:10.
Heating the condition that boiling is handled in step 1), in compressive reaction kettle is：Heating-up time 1h, maximum temperature be 120~
150 DEG C, soaking time is 1~4h, and the condition that boiling processing is heated in normal-pressure reaction kettle is：Maximum temperature is 110~140 DEG C,
Soaking time is 3~12h.
In step 2), the cleaning solution is acetone, ethyl alcohol or water.
In step 4), it is 200 dalton that the NF membrane in the nanofiltration separation, which stays molecular weight,.
In step 4), cycling and reutilization after the concentrated dehydration of eutectic solvent aqueous solution.
Advantageous effect：Compared with prior art, remarkable advantage of the invention is：
1) present invention provides a kind of green nothing using the method for eutectic solvent heating boiling processing plant fiber material
It is useless to eliminate chemical steaming in traditional fibre element, hemicellulose and lignin separation for pollution, eutectic solvent can be recycled
Pollution of the liquid to environment, realize three component of plant fiber material efficiently separate and recycling.
2) present invention uses but is not limited to traditional heating boiling treatment process, and the technique can realize plant fiber original
Material each component is sufficiently separated, and it is more than the cellulose that the 79.5%, degree of polymerization is up to 1113 to obtain chemical cellulose content, and purity is more than
89% lignin and yield is more than 45% hemicellulose, and energy consumption is low, and gained size performance is excellent, and there is industrialization to answer
Use foreground.
Specific implementation mode
Below in conjunction with the technical matters step in the embodiment of the present invention, condition and material is embodied, to of the invention real
The technical solution applied in example is clearly and completely described, it is clear that described embodiment is only that a present invention part is implemented
Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not paying creativeness
The every other embodiment obtained under the premise of labour, shall fall within the protection scope of the present invention.
Embodiment 1
The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material, specific steps are such as
Under：
1) lactic acid/choline chloride eutectic solvent configuration
Extracting lactic acid and choline chloride mixing, 1h is stirred at 60 DEG C, and it is 9 to be configured to molar ratio:1 lactic acid/choline chloride
Eutectic solvent.
2) plant fiber material heats boiling processing in eutectic solvent
Long 2~4cm, wide 1~2cm poplar piece place 2 days in air after, measure moisture, weigh over dry 50g poplar pieces
The 250g molar ratios for being added in compressive reaction kettle, and step 1) preparation being added are 9:1 lactic acid/choline chloride eutectic is molten
Agent, it is 1 to make the solid-to-liquid ratio of plant fiber material and eutectic solvent:5, then carry out heating boiling processing.Heat boiling processing
Condition be：Heating-up time is 1h, and 150 DEG C, soaking time 2h of holding temperature obtains eutectic after the completion of heating boiling processing
Solvent treated mixture.
3) separation of cellulose (slurry)
Eutectic solvent treated the mixture that step 2) obtains is washed after strainer squeezes filtering with acetone, through filtering
Solid portion after washing is that slurry (cellulose) takes part to measure its yield, Kappa number, the degree of polymerization and chemical cellulose after air-drying
Content etc. collects filtered fluid and acetone cleaning solution.
4) separation of lignin
The acetone cleaning solution that step 3) obtains is collected acetone and is recycled, remaining liq is added step 3) and obtains by revolving
Filtered fluid, be added dropwise to together in a large amount of water (volume ratio be more than 10:1), lignin settles out, and centrifuges, and solid portion is
Lignin measures its yield and lignin purity after drying, collects centrifuged supernatant part.
5) separation of hemicellulose
It is receiving for 200 dalton through nanofiltration retaining molecular weight after the concentrated dehydration of centrifuged supernatant that step 4) obtains
Filter separation, solid portion obtain hemicellulose, the concentrated dehydration of eutectic solvent aqueous solution of liquid portion after dehydration and drying
Cycling and reutilization afterwards.
Embodiment 2
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, wherein
In step 2), plant fiber material sample grows the poplar piece of 2~4cm wide, 1~2cm using the masson pine of 1~2cm of long 2~4cm wide
The masson pine wood powder of the mesh of the poplar wood powder of the mesh of wood chip, the moso bamboo bamboo chip of long 2~4cm wide, 1~2cm, 20 mesh~80,20 mesh~80,
Any replacement of wheat straw of the moso bamboo bamboo powder of the mesh of 20 mesh~80, the straw of long 2~4cm, long 2~4cm.
Embodiment 3
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, wherein
In step 2), molar ratio 9:1 lactic acid/choline chloride eutectic solvent uses molar ratio for 5:1、7:1、11:1 lactic acid/chlorine
Change any replacement of choline.
Embodiment 4
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, wherein
In step 2), the solid-to-liquid ratio of plant fiber material and eutectic solvent is 1:5 use solid-to-liquid ratio for 1:3、1:7、1:10 is any
It substitutes.
Embodiment 5
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, wherein
In step 2), the condition of heating boiling processing：150 DEG C of holding temperature is protected using 120 DEG C, 130 DEG C, 140 DEG C of any replacements
Warm time 2h uses any replacement of 1h, 3h, 4h.
Embodiment 6
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, step
1), 3), 4), 5) with embodiment 1, in step 2), compressive reaction kettle is substituted with normal-pressure reaction kettle, and plant fiber material is in eutectic
It is as follows that boiling processing is heated in solvent：Long 2~4cm, wide 1~2cm poplar piece place 2 days in air after, measure moisture, claim
The 250g molar ratios for taking over dry 50g poplar pieces to be added in normal-pressure reaction kettle, and step 1) preparation being added are 9:1 lactic acid/chlorine
Change choline eutectic solvent, it is 1 to make the solid-to-liquid ratio of plant fiber material and eutectic solvent:5, then carry out heating boilery
Reason.Heating the condition that boiling is handled is：150 DEG C, soaking time 10h of holding temperature obtains low total after the completion of heating boiling processing
Molten solvent treated mixture.
Embodiment 7
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 6, wherein
In step 2), the condition of heating boiling processing：150 DEG C of holding temperature is protected using 120 DEG C, 130 DEG C, 140 DEG C of any replacements
Warm time 10h uses any replacement of 6h, 12h.
Embodiment 8
The separation of three component of cellulose, hemicellulose and lignin in plant fiber material, method is the same as embodiment 1, wherein
In step 3), cleaning solution acetone is using ethyl alcohol, any replacement of water.
Cellulose (slurry), lignin and hemicellulose analysis to being obtained in embodiment 1-8, the results are shown in Table 1.
Cellulose (slurry), lignin and the hemicellulose analysis result that table 1 obtains
Note：Cellulose (slurry) yield is the yield of relative raw material, lignin yield be in relative raw material lignin
Rate, the yield of hemicellulose are the yield of hemicellulose in relative raw material.2 result of embodiment is using 1~2cm of long 2~4cm wide
Masson pine wood chip；3 result of embodiment is to use the molar ratio of lactic acid/choline chloride for 11:1；4 result of embodiment is using solid
Liquor ratio is 1:7；5 result of embodiment is the soaking time 4h using 120 DEG C；7 result of embodiment is the soaking time using 140 DEG C
12h；8 result of embodiment is using ethyl alcohol.
As it can be seen from table 1 pulp yield relative to raw material up to 57.5%, slurry of the Kappa number 13.0 can be obtained, gather
Right to reach 1113, chemical cellulose content is up to 85.5%.Lignin yield is reached relative to raw material wood element amount
64.9%, and its purity relatively up to 97.5%.Hemicellulose yield relative to raw material hemicellulose quality up to 56.1%, hemicellulose
Xylan content is up to 93.2% in element.
Claims (8)
1. the separation method of three component of cellulose, hemicellulose and lignin in a plant fiber raw material, which is characterized in that packet
Include following steps：
1) lactic acid of preparation/choline chloride eutectic solvent is added to the plant fiber material air-dried after crushing, solid-liquid is mixed
Object, which is added in compressive reaction kettle or normal-pressure reaction kettle, carries out heating boiling processing, obtains eutectic solvent treated mixture；
2) by the eutectic solvent being prepared in step 1) treated mixture after strainer squeezes filtering, washed liquid is washed
It washs to obtain insoluble matter cellulose and the eutectic solvent dissolution fluid containing hemicellulose and lignin；
3) by the eutectic solvent dissolution fluid containing hemicellulose and lignin of gained in step 2) it is concentrated after, be added to the water again
Raw isolated lignin and the eutectic solvent aqueous solution containing hemicellulose；
4) half will be obtained by nanofiltration separation after eutectic solvent aqueous solution thickening of the gained containing hemicellulose in step 3)
Cellulose.
2. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 1), used lactic acid and choline chloride eutectic solvent molar ratio are 3~15:1.
3. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 1), plant fiber material is needlebush, leaf wood, bamboo material or grass raw material, plant
Fibrous raw material crush after size include the particle of the mesh of 20 mesh~80, the wood chip of 1~2cm of long 2~4cm wide or bamboo chip, it is long by 2~
The grass raw material of 4cm.
4. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 1), the solid-to-liquid ratio of used plant fiber material and eutectic solvent is 1:3~1:10.
5. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：Heating the condition that boiling is handled in step 1), in compressive reaction kettle is：Heating-up time 1h, maximum temperature are
120~150 DEG C, soaking time is 1~4h, and the condition that boiling processing is heated in normal-pressure reaction kettle is：Maximum temperature be 110~
140 DEG C, soaking time is 3~12h.
6. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 2), the cleaning solution is acetone, ethyl alcohol or water.
7. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 4), it is 200 dalton that the NF membrane in the nanofiltration separation, which stays molecular weight,.
8. the separation side of three component of cellulose, hemicellulose and lignin in plant fiber material according to claim 1
Method, it is characterised in that：In step 4), cycling and reutilization after the concentrated dehydration of eutectic solvent aqueous solution.
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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 |
| CN110540508A (en) * | 2019-08-30 | 2019-12-06 | 齐鲁工业大学 | Eutectic solvent and application thereof in extracting lignin |
| CN111359258A (en) * | 2020-03-06 | 2020-07-03 | 哈尔滨工业大学（威海） | Novel system for separating and purifying hydrophobic eutectic solvent of weak protonic acid and method for purifying weak protonic acid |
| CN111592680A (en) * | 2020-06-15 | 2020-08-28 | 齐鲁工业大学 | High-water-absorptivity aerogel packaging material prepared from reed waste residues and preparation method thereof |
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