CN106854842B - A kind of technique of synchronously producing cellulosic element nano whisker and ethyl alcohol - Google Patents
A kind of technique of synchronously producing cellulosic element nano whisker and ethyl alcohol Download PDFInfo
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- CN106854842B CN106854842B CN201710034698.2A CN201710034698A CN106854842B CN 106854842 B CN106854842 B CN 106854842B CN 201710034698 A CN201710034698 A CN 201710034698A CN 106854842 B CN106854842 B CN 106854842B
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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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/06—Ethanol, i.e. non-beverage
- C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
- C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
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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
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- D21C3/22—Other features of pulping processes
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- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
The invention discloses the techniques of a kind of synchronously producing cellulosic element nano whisker and ethyl alcohol.Its technological process is：Stock → PFI mashing → Concentrated acid hydrolysis → centrifuge washing → suspension → dialysis → Cellulose nanocrystal palpus（CNC）;Centrifuged supernatant+residue → CaCO3Adjust pH → dilute acid hydrolysis → CaCO3Neutralization reaction → micro porous filtration → common fermentation → bio-ethanol.It is an advantage of the invention that the utilization rate of raw material is high, ethanol conversion is high, and contaminated wastewater is few, and a new way is provided for biomass efficient high level conversion.
Description
Technical field
It is fine more particularly, to a kind of synchronous production the present invention relates to Cellulose nanocrystal palpus (CNC) and alcohol production field
The plain nano whisker (CNC) of dimension and the technique of ethyl alcohol.
Background technology
Native cellulose is biomass resource most abundant in nature, is widely present in animal, plant and microorganism.
Cellulose is the wire macromolecule with crystalline texture being formed by connecting by β-D- glucopyranoses units with 1,4- β-glycosidic bond
Compound.In general, Cellulose nanocrystal palpus (CNC) is mainly the length being made of the crystal region of cellulose in 50-400nm
Between, diameter between 10-30nm, the rodlike aggregated structure of high-crystallinity.These characteristics cause nano micro crystal cellulose
With very high economic value, nanocomposite, medical carrier, papermaking, packaging, coating, food additives etc. are widely used in
Field.
For at present, CNC preparation methods the most universal hydrolyze for the concentrated sulfuric acid, and yield is about between 20-50%.This
Mean that most cellulose and hemicellulose are present in the form of oligosaccharide in CNC waste liquids.These carbohydrates are with waste water
Discharge causes the waste of resource.Therefore, it is one feasible efficiently using biomass resource to prepare bio-ethanol using CNC waste water
Approach, although there are many problems for it.First, CNC waste water contains substantial amounts of sulfuric acid, with can generate high-salt wastewater after alkali neutralization.
2nd, the most of Efficient Conversion for existing in the form of oligosaccharide, influencing ethyl alcohol of sugar in waste water.3rd, given birth to conventional fibre raw material
There are substantial amounts of xylans in the waste water of production CNC not to be utilized.
The content of the invention
The object of the present invention is to provide the techniques of a kind of synchronously producing cellulosic element nano whisker and ethyl alcohol.Advantages of the present invention
It is that the utilization rate of raw material is high, ethanol conversion is high, and contaminated wastewater is few, and a new way is provided for biomass efficient high level conversion
Footpath.
The purpose of the present invention is what is realized by following technical method.
The technique of a kind of synchronously producing cellulosic element nano whisker and ethyl alcohol, comprises the following steps：
(1) stock up：It is torn up after pulpboard is impregnated；
(2) it is beaten：Pulpboard after tearing up is added in PFI mills and is beaten, and re-dry obtains slurry；
(3) Concentrated acid hydrolysis：Concentrated acid is added in into slurry obtained by step (2), reaction is hydrolyzed at 40-60 DEG C, after reaction
It adds in water and terminates reaction；
(4) centrifuge washing：Centrifugation, collects supernatant, and constantly repeats to add water washing into solid residue, centrifugation, in collection
Clear liquid, until supernatant becomes cloudy, then the turbid solution on collection upper strata, continues into solid residue plus water rinses, centrifuge, collect
The turbid solution on upper strata is clarified until upper strata turbid solution becomes, regathers solid residue；
(5) dialyse：Turbid solution obtained by step (4) is added in bag filter and is dialysed, obtains Cellulose nanocrystal palpus；
(6) pH is adjusted：Supernatant and solid residue obtained by blend step (4) adjust the pH to 0.15-0.2 of acquired solution；
(7) dilute acid hydrolysis：By dilute acid hydrolysis in step (6) acquired solution addition autoclave 115-125 DEG C, must hydrolyze
Liquid；
(8) neutralization reaction：The pH of hydrolyzate is adjusted as neutrality；
(9) filter：By mixed liquor filtering obtained by step (8), filtrate and filter residue are obtained；
(10) anaerobic fermentation：Fermented nutritive liquid and yeast extract are added in filtrate obtained by step (9), obtain zymotic fluid,
Anaerobic fermentation 48-96h is carried out at 30-40 DEG C again, obtains ethyl alcohol.
Preferably, step (1) described pulpboard not dissolves pulpboard for common pulpboard.
Preferably, step (3) described concentrated acid be sulfuric acid, concentration 60-64wt%.
Preferably, the mass ratio of step (3) slurry and concentrated acid is 1:15-1:30；The time of the hydrolysis is
30-90min；The dosage of the water is 5-10 times of reaction solution volume.
Preferably, the water frequency of changing of step (5) described dialysis is 2-3 times/day, and dialysis time is 5-7 days, the rule of bag filter
Lattice are 7000-12000Da.
Preferably, step (6) is with adjusting substance used in pH as grinding CaCO in step (8)3。
Preferably, the condition of step (7) described dilute acid hydrolysis is：PH=0.15-0.2, reaction time 40-120min.
Preferably, step (10) described fermented nutritive liquid is (NH4)2SO4、KH2PO4、MgSO4、CaCl2With the mixing of water
Liquid；(the NH4)2SO4、KH2PO4、MgSO4、CaCl2It is respectively 0.5-1.5g/ with concentration of the yeast extract in zymotic fluid
L, 2-3g/L, 0.3-0.5g/L, 0.05-0.15g/L and 0.25-0.75g/L.
Preferably, step (10) described anaerobic fermentation keeps the temperature program using gradient, concretely comprises the following steps：First in 37-40 DEG C of guarantor
24-36h is held, then 48-72h is kept at 28-30 DEG C.
Preferably, step (10) described yeast extract is saccharomyces cerevisiae CICC1416 and shehatae candida
GIM2.175。
Compared with prior art, the present invention has following technique effect：
1st, the present invention can synchronously obtain the Cellulose nanocrystal palpus of high quality and high sugared waste water using two-stage acid hydrolysis method, have
Effect improves the utilization rate of raw material.
2nd, the present invention utilizes and grinds CaCO3Sugared waste water high to gained carries out neutralization reaction, then carries out micro porous filtration, effectively
Avoid a large amount of accumulation of inorganic salts in waste water.
3rd, the present invention converts the high sugared waste water of gained using five hexose common fermentations, and monose utilization rate is high, and ethanol conversion is good,
A new way is provided for biomass efficient high level conversion.
Description of the drawings
Fig. 1 is the XRD spectra and crystallinity of the CNC prepared under different acid hydrolysis conditions.
Fig. 2 is the size analysis chart of the CNC prepared under different acid hydrolysis conditions.
Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d are the TEM pictures of the CNC prepared under different acid hydrolysis conditions respectively.
Specific embodiment
Below by way of attached drawing and example, the invention will be further described, but the implementation of the present invention is not limited to this.
Embodiment 1
(1) stock up：30g poplars pulpboard is added in 0.5L water after impregnating 4h and torn up；
Poplar pulpboard used in the present embodiment comes from Shandong Province of China slurry factory, into being grouped into and essential element composition is such as table 1
It is shown.
Table 1
(2) it is beaten：Pulpboard after tearing up adds in mashing in PFI mills (Mark V1 types)；Conditions of beating is：Slurry concentration：
10wt%, beating pressure：3.33N/mm blade lengths；Revolution：2000 turns.After the completion of mashing, slurry is placed in 40 DEG C of vacuum and is done
In dry case overnight, slurry is obtained.
(3) Concentrated acid hydrolysis：The concentrated sulfuric acid is added in into slurry obtained by step (2), reaction is hydrolyzed, reaction is added in after reaction
The water of 5 times of volumes of liquid terminates reaction；
The present embodiment must be with high sugared waste water, process conditions such as table using two step sulphuric acid hydrolysis production Cellulose nanocrystal
Shown in 2.
Table 2
(4) centrifuge washing：Centrifugation, collects supernatant, and constantly repeats to add water washing into solid residue, centrifugation, in collection
Clear liquid, until supernatant becomes cloudy, then the turbid solution on collection upper strata, continues into solid residue plus water rinses, centrifuge, collect
The turbid solution on upper strata is clarified until upper strata turbid solution becomes, regathers solid residue；Centrifugal condition is：Centrifugal force：1200g, every time
Centrifugation time：10min；
(5) dialyse：Turbid solution obtained by step (4) is added in the bag filter of 7000Da and dialyse 5 days, change water frequency be 2 times/
My god, obtain Cellulose nanocrystal palpus (CNC)；
(6) pH is adjusted：All supernatant and solid residue obtained by blend step (4), with grinding CaCO3It is molten to adjust gained
The pH of liquid to 0.18；
(7) dilute acid hydrolysis：By step (6) acquired solution (pH=0.18) loaded in sterilizing bottle, it is placed in 121 in autoclave
Dilute acid hydrolysis 60min at DEG C, obtains hydrolyzate；
(8) neutralization reaction：With grinding CaCO3The pH of hydrolyzate is adjusted as neutrality；
(9) filter：Mixed liquor obtained by step (8) with millipore filter is filtered, obtains filtrate and filter residue；The hole of miillpore filter
Footpath is 0.45 μm；
(10) anaerobic fermentation：Fermented nutritive liquid and yeast extract are added in filtrate obtained by step (9), obtain zymotic fluid,
Then first kept for 24 hours at 40 DEG C in fermentation tank, then 48h is kept at 30 DEG C, obtain ethyl alcohol；The fermented nutritive liquid is (NH4)2SO4、KH2PO4、MgSO4、CaCl2With the mixed liquor of water；(the NH4)2SO4、KH2PO4、MgSO4、CaCl2And yeast extract
Concentration in zymotic fluid is respectively 1g/L, 2.5g/L, 0.4g/L, 0.1g/L and 0.5g/L；The yeast extract is wine brewing
Yeast CICC1416 and shehatae candida GIM2.175 (mass ratio=1:1)
The present embodiment utilizes crystallization of the x-ray diffractometer (D8ADVANCE, German Bruker companies) to obtained NCC
Structure is analyzed.XRD test conditions are：Cu targets, pipe press 40KV, electric current 40mA, 35.4 seconds/step of sweep speed, step-length 0.04
Degree, scanning range 5-60 degree.Gained XRD spectrum is as shown in Figure 1.
As shown in Figure 1, using poplar pulpboard as raw material, CNC prepared by different acid hydrolysis conditions has typical cellulose Ⅰ
The structure of type.The crystallinity of CNC substantially increases with the increase in Concentrated acid hydrolysis reaction time, shows with acid hydrolytic reaction
The noncrystalline domain for carrying out cellulose is constantly destroyed.CNC crystallinity obtained by the present embodiment is between 64.5-67.5%.Greatly
Quantity research shows that CNC crystallinity is higher, and the intensity of gained cellulosic material is bigger.
The present embodiment is using Laser Scattering Particle Size Distribution Analyzer (LA-960S, Japanese HORIBA companies) to the size of CNC
Size is analyzed.Acquired results are as shown in Figure 2.
As shown in Fig. 2, the CNC grain sizes obtained by the present embodiment are nanoscale, average grain diameter is between 276-467nm.
Obtained CNC average grain diameters substantially reduce with the increase of sour hydrolysis degree.It is obtained when the sulphuric acid hydrolysis time is 80min
The minimum 276nm of average grain diameter of CNC.
The present embodiment carries out the CNC obtained by different acid hydrolysis conditions using Flied emission transmission electron microscope (JEM-2100F)
Exterior appearance is analyzed, and result is as shown in Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d.
As shown in Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d, #1, #3, #4 and #6 sample are that length is 200-400nm or so, directly
The club shaped structure of footpath 10-30nm or so.In addition, with the increase of sour hydrolysis time, the size of cellulose becomes evenly.This reality
Apply the exterior appearance that the product obtained by example complies fully with commodity CNC.
The present embodiment analyzes the saccharic composition of CNC waste liquids using ion chromatography (Dionex ICS-5000).IC is detected
Condition is：Detector：Dionex IonPacTMAG11-HC, chromatographic column：Dionex CarboPac PA20, mobile phase：
2mmol/L NaOH, flow velocity：0.5mL/min, eluent：200mmol/L NaOH and 1mol/L NaAC.Its testing result such as table
Shown in 3.
Table 3
Unit：g/L
| Title | #1 | #2 | #3 | #4 | #5 | #6 |
| Glucose | 0.55 | 1.08 | 1.28 | 1.35 | 2.67 | 2.10 |
| Xylose | 2.41 | 2.45 | 2.41 | 1.91 | 2.75 | 2.21 |
| Mannose | 0 | 0 | 0 | 0 | 0 | 0.23 |
| Ligoglucoside | 1.93 | 2.51 | 2.01 | 1.48 | 2.15 | 1.37 |
| Wood oligose | 0.87 | 1.13 | 0.69 | 1.15 | 0.57 | 0.77 |
| Manna oligosacchride | 0.64 | 0.89 | 0.54 | 0.51 | 0.69 | 0.35 |
| Monose | 2.97 | 3.53 | 3.70 | 3.27 | 5.45 | 4.55 |
| Oligosaccharide | 3.46 | 4.54 | 3.27 | 3.17 | 3.42 | 2.49 |
As shown in table 3, simultaneously containing substantial amounts of monose and oligosaccharide in the acid hydrolysis liquid of poplar slurry, this is because fiber
The sour water solution of element and hemicellulose firstly generates oligosaccharides, is then further hydrolyzed to monose.Therefore, in the production process of CNC
In, relatively low reaction temperature makes carbohydrate largely be present in CNC waste liquids in the form of oligosaccharides.This part in the present embodiment
Oligosaccharides can further be degraded to monose during secondary dilute acid hydrolysis, so as to increase the fermentable sugars concentration of mash.
Table 4
Unit：Kg/t pulpboards
| Group | NCC | Ethyl alcohol |
| #1 | 90 | 155 |
| #2 | 199 | 129 |
| #3 | 249 | 149 |
| #4 | 506 | 124 |
| #5 | 414 | 106 |
| #6 | 496 | 97 |
The present embodiment utilizes saccharomyces cerevisiae (CICC1416) and shehatae candida (GIM2.175) co-fermentation technology pair
The sugared waste liquids of CNC high under different acid hydrolysis conditions ferment.Table 4 is the MaterialBalance Computation of the present embodiment.As shown in Table 4,
Using poplar pulpboard be raw material, acid hydrolysis conditions 60wt%H2SO4, 60min, pulpboard per ton can produce simultaneously 506kg CNC and
124kg ethyl alcohol.
It is above the desirable embodiment of the present invention, those skilled in the art completely can be without departing from this invention technological thought
In the range of, carry out a variety of modifications and optimization.And these all modifications and optimization are included in such as the claims in the present invention institute
The Spirit Essence included within the scope of restriction without departing from the present invention and required practical scope.
Claims (7)
1. the technique of a kind of synchronously producing cellulosic element nano whisker and ethyl alcohol, which is characterized in that comprise the following steps：
（1）Stock：It is torn up after pulpboard is impregnated；
（2）Mashing：Pulpboard after tearing up is added in PFI mills and is beaten, and re-dry obtains slurry；
（3）Concentrated acid hydrolysis：To step（2）Concentrated acid is added in gained slurry, reaction is hydrolyzed at 40-60 DEG C, is added in after reaction
Water terminates reaction；The mass ratio of the slurry and concentrated acid is 1: 15-1:30；The time of the hydrolysis is 30-90 min；
The dosage of the water is 5-10 times of reaction solution volume；
（4）Centrifuge washing：Centrifugation, collects supernatant, and constantly repeats into solid residue plus water washing, centrifugation collect supernatant,
Until supernatant becomes cloudy；Then the turbid solution on upper strata is collected, continues into solid residue plus water rinses, upper strata is collected in centrifugation
Turbid solution, until upper strata turbid solution become clarify, regather solid residue；
（5）Dialysis：By step（4）Gained turbid solution is added in bag filter and dialysed, and obtains Cellulose nanocrystal palpus；
（6）Adjust pH：Blend step（4）Gained all supernatant and solid residue adjust the pH to 0.15- of acquired solution
0.2；
（7）Dilute acid hydrolysis：By step（6）Dilute acid hydrolysis at 115-125 DEG C, obtains hydrolyzate in acquired solution addition autoclave；Institute
The condition for stating dilute acid hydrolysis is：PH=0.15-0.2, reaction time 40-120min；
（8）Neutralization reaction：The pH of hydrolyzate is adjusted as neutrality；
（9）Filtering：By step（8）Gained mixed liquor filters, and obtains filtrate and filter residue；
（10）Anaerobic fermentation：Fermented nutritive liquid and yeast extract are added in into step（9）In gained filtrate, zymotic fluid is obtained, then
Anaerobic fermentation 48-96h is carried out at 30-40 DEG C, obtains ethyl alcohol；The fermented nutritive liquid is (NH4)2SO4、 KH2PO4、 MgSO4、
CaCl2With the mixed liquor of water；The yeast extract is saccharomyces cerevisiae CICC1416 and shehatae candida GIM2.175.
2. technique according to claim 1, which is characterized in that step（1）The pulpboard is not dissolving pulp for common pulpboard
Plate.
3. technique according to claim 1, which is characterized in that step（3）The concentrated acid be sulfuric acid, concentration 60-
64wt%。
4. technique according to claim 1, which is characterized in that step（5）The dialysis changes water frequency as 2-3 times/day,
Dialysis time is 5-7 days, and the specification of bag filter is 7000-12000 Da.
5. technique according to claim 1, which is characterized in that step（6）With step（8）It is middle adjusting pH used in substance be
Grind CaCO3。
6. technique according to claim 1, which is characterized in that step（10）(the NH4)2SO4、 KH2PO4、 MgSO4、
CaCl2It is respectively 0.5-1.5g/L, 2-3g/L, 0.3-0.5g/L, 0.05- with concentration of the yeast extract in zymotic fluid
0.15g/L and 0.25-0.75g/L.
7. technique according to claim 1, which is characterized in that step（10）The anaerobic fermentation keeps the temperature journey using gradient
Sequence concretely comprises the following steps：24-36 h are first kept at 37-40 DEG C, then 48-72 h are kept at 28-30 DEG C.
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| CN111395031A (en) * | 2020-03-23 | 2020-07-10 | 华南理工大学 | Method for synchronously preparing cellulose nanowhiskers and cellulose nanofibrils |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304550A (en) * | 2011-10-10 | 2012-01-04 | 山东大学 | Method for producing ethanol or acetone and butanol by taking lignocellulose as raw material |
| CN103740768A (en) * | 2013-12-31 | 2014-04-23 | 朱江 | Full resource biological utilization process of lignocellulose material |
| CN104031946A (en) * | 2013-03-06 | 2014-09-10 | 国网新源控股有限公司北京非粮醇电联产技术研发中心 | Detoxification treatment-free cellulosic ethanol production method |
| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304550A (en) * | 2011-10-10 | 2012-01-04 | 山东大学 | Method for producing ethanol or acetone and butanol by taking lignocellulose as raw material |
| CN104031946A (en) * | 2013-03-06 | 2014-09-10 | 国网新源控股有限公司北京非粮醇电联产技术研发中心 | Detoxification treatment-free cellulosic ethanol production method |
| CN103740768A (en) * | 2013-12-31 | 2014-04-23 | 朱江 | Full resource biological utilization process of lignocellulose material |
| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
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