CN107501357A - A kind of cellulose fermentable sugars and preparation method and application - Google Patents
A kind of cellulose fermentable sugars and preparation method and application Download PDFInfo
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- CN107501357A CN107501357A CN201710645675.5A CN201710645675A CN107501357A CN 107501357 A CN107501357 A CN 107501357A CN 201710645675 A CN201710645675 A CN 201710645675A CN 107501357 A CN107501357 A CN 107501357A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a kind of cellulose fermentable sugars and preparation method and application.This method comprises the following steps：(1) it is 1 in mass ratio by the mixed solution of jute pulp and sodium hydroxide and urea：Stirred after 40~60 mixing, obtain mixed system；(2) mixed system obtained in step (1) is cooled to 8~12 DEG C, stirring and dissolving, obtains cellulose solution；(3) cellulose solution in step (2) is subjected to neutralisation treatment, concentration, is then 1 by volume by the cellulose solution after concentration and dilution heat of sulfuric acid：4~12 mixing, carry out sour water solution, obtain cellulose fermentable sugars.Instant invention overcomes required sour concentration present in the cellulolytic method of classical acid is big, it is dangerous big and to equipment corrosion it is serious the problem of, using simpler, efficient method acid saccharification cellulose and hemicellulose, obtained cellulose fermentable sugars can be used for producing bio-ethanol.
Description
Technical field
The invention belongs to fibrous material applied technical field, more particularly to a kind of cellulose fermentable sugars and preparation method thereof
With application.
Background technology
As fossil fuel by shortage becomes exhausted, energy crisis turns into the common issue of facing mankind.Find new energy
Concern the sustainable development of economy and the tremendous development of the mankind in source.In various regenerative resources, biomass is unique, only
One reproducible carbon source, conventional solid-state, liquid or gaseous fuel can be converted into.Moreover, biomass source is in air
H2O and CO2, H is regenerated after burning2O and CO2, so CO in air will not be increased2Content.Therefore, with mineral matter energy phase
Than biomass energy is a kind of energy more cleaned.
Although China takes much count of the research and technological development of Production of Alcohol from Lignocellulose now, skill is all suffered from
The huge challenge of art and economic aspect.At present, the method for hydrolysis of lignocellulosic mainly has two kinds of Acid hydrolysis and enzymatic hydrolysis
Method.Acid hydrolysis is although higher glucose yield can be obtained, but concentrated acid not only produces larger corrosion to equipment, and
Contain the hydrolysate that suppression is largely produced to microorganism in hydrolyzate so that final alcohol fermentation is less efficient.It is in addition, fine
Tie up that plain production of enzyme is low, unstable property also increases the difficulty that enzyme process prepares bio-ethanol.It is existing in order to solve the problems, such as, it is anxious
A kind of new mode need to be found and prepare cellulose fermentable sugars.
The content of the invention
The shortcomings that primary and foremost purpose of the present invention is to overcome prior art and deficiency, there is provided a kind of cellulose fermentable sugars
Preparation method.
The cellulose fermentable sugars being prepared another object of the present invention is to provide methods described.
A further object of the present invention is the application for providing the cellulose fermentable sugars.
The purpose of the present invention is achieved through the following technical solutions：A kind of preparation method of cellulose fermentable sugars, including with
Lower step：
(1) it is 1 in mass ratio by jute pulp and sodium hydroxide/urea mixed solution：Stir, mixed after 40~60 mixing
System；
(2) mixed system obtained in step (1) is cooled to -8~-12 DEG C, stirring and dissolving, obtains cellulose solution；
(3) cellulose solution in step (2) is subjected to neutralisation treatment, concentration, then by the cellulose solution after concentration
It is 1 by volume with dilution heat of sulfuric acid：4~12 mixing, then sour water solution is carried out, obtain cellulose fermentable sugars.
Jute pulp described in step (1) is the raw material containing cellulose, hemicellulose, lignin and other materials；It is preferred that
For known fiber element and hemicellulose level over dry jute pulp because fermentable sugars is obtained by cellulose and hemicellulose degradation
, therefore cellulose and the content of hemicellulose in known slurry, the yield of fermentable sugars can be calculated.
Sodium hydroxide/urea mixed solution described in step (1) is the hydrogen for being mixed to get sodium hydroxide, urea and water
The mixed solution of sodium oxide molybdena and urea.
The mass fraction 5~10% of sodium hydroxide in mixed system described in step (1), the mass fraction 3 of urea~
15%.
It is cooled to carry out under air-proof condition described in step (2), avoids the carbon dioxide and sodium hydroxide in air
Reaction.
The speed of stirring described in step (2) is preferably 3000~9000r/min.
The time of stirring described in step (2) is preferably 5~10min.
Neutralisation treatment described in step (3) is to adjust PH to neutrality using hydrochloric acid solution.
The molar concentration of described hydrochloric acid solution is preferably 5~8mol/L.
Concentration described in step (3) is to be concentrated using Rotary Evaporators；Rotary Evaporators are preferably used by fibre
It is 6~10g/L to tie up plain solution and be concentrated into concentration.
The dilution heat of sulfuric acid that adds described in step (3) is slowly to add under 6000~9000r/min high shear
Enter dilution heat of sulfuric acid.
The concentration of dilution heat of sulfuric acid described in step (3) is mass percent 4%.
Acid-hydrolyzed condition described in step (3) is preferably：1h is hydrolyzed under the conditions of 120 DEG C.
A kind of cellulose fermentable sugars, is prepared by the method described in any of the above-described.
Application of the described cellulose fermentable sugars in bio-ethanol field.
The present invention is had the following advantages relative to prior art and effect：
1st, the present invention presses jute pulp and sodium hydroxide/urea mixed solution of known fiber element and hemicellulose level certain
Mass ratio mixing, stirring, form uniform mixed system, and dissolve solid fabric element under certain condition, form it into easily
In acid-hydrolyzed cellulose solution, then with the dilute sulfuric acid that mass fraction is 4% acidification hydrolization cellulose under certain condition, system
Obtain the cellulose fermentable sugars that can be used for production bio-ethanol.Instant invention overcomes deposited in the cellulolytic method of classical acid
Required sour concentration it is big, it is dangerous big and to equipment corrosion it is serious the problem of, while also avoid using cellulase, solve
The problem of cost is high in enzyme hydrolysis cellulose method, and efficiency is low.
2nd, the species of slurry has large effect to solubility of the cellulose in sodium hydroxide/urea mixed solution, slurry
Expect that the solubility in mixed solution can further influence the effect of acidolysis again.Present invention selection ramie pulp fiber as raw material, by
The condition of other auxiliary agents is being increased without with regard to that can reach the features such as ramie pulp fiber its own hemicellulose level is low, the degree of polymerization is small
Nearly 100% solute effect, reduce influence of the solid fiber to effect of sulfuric acid effect, improve the effect of acidolysis fiber.
3rd, the dilute sulfuric acid in the present invention is to be slowly added into cellulose solution under 6000~9000r/min high shear force
In, acidolysis is then carried out, is because the addition of acid can neutralize the hydroxyl in cellulose solution, makes the part of dissolving cellulose again
It is raw.And the regenerated cellulose crystallinity formed is relatively low, intensity difference, and more fiber fines be present, high shear is on the one hand
The generation of regenerated cellulose can be limited, on the other hand can also destroy the regenerated cellulose of generation, increases sulfuric acid and cellulose
Contact area, promote cellulose acidolysis into monose.
4th, the concentration of present invention selection suitable acid-hydrolyzed temperature, time and sulfuric acid, can be reduced under this condition
The generation of inhibitor, facilitates monose to ferment in acid hemolysis process.
5th, the acid saccharification efficiency high of cellulose and hemicellulose in the present invention, maximum acidolysis saccharification efficiency is respectively 87%
With 98% (relative to theoretical value).
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Agents useful for same in the embodiment of the present invention is commercially available.
Embodiment 1：The preparation of cellulose fermentable sugars
(1) take 7g known fibers element and hemicellulose level be respectively 95.33% and 1.73% over dry jute pulp and hydrogen-oxygen
It is 1 in mass ratio to change sodium and urea mixed solution:40 mixing, stirring, form uniform mixed system；Wherein, in mixed system
The mass fraction of sodium hydroxide and urea is respectively 5% and 3%.
(2) by mixed system under sealed conditions (system be fully sealed be in order to avoid the carbon dioxide in air with
Sodium hydroxide reacts) -8 DEG C are cooled to, and 5min is stirred under conditions of 3000r/min, obtain cellulose solution.
(3) hydrochloric acid solution for taking cellulose solution to be first 6mol/L with molar concentration adjusts PH to neutrality, then rotated steaming
The concentration that hair instrument is concentrated into cellulose solution is 6g/L, then by the fiber after concentration under 6000r/min high shear
The dilution heat of sulfuric acid that plain solution is 4% with mass fraction is 1 by volume:4 mixing, form mixed liquor；Finally by the mixed liquor
High-temperature acid hydrolyzes 1h under the conditions of 120 DEG C, makes cellulose monose, that is, obtains cellulose fermentable sugars.
Embodiment 2：The preparation of cellulose fermentable sugars
(1) take 7g known fibers element and hemicellulose level be respectively 95.33% and 1.73% over dry jute pulp and hydrogen-oxygen
It is 1 in mass ratio to change sodium and urea mixed solution:50 mixing, stirring, form uniform mixed system；Wherein, in mixed system
The mass fraction of sodium hydroxide and urea is respectively 7% and 7%.
(2) by mixed system under sealed conditions (system be fully sealed be in order to avoid the carbon dioxide in air with
Sodium hydroxide reacts) -9 DEG C are cooled to, and 7min is stirred under conditions of 5000r/min, obtain cellulose solution.
(3) hydrochloric acid solution for taking cellulose solution to be first 6mol/L with molar concentration adjusts PH to neutrality, then rotated steaming
The concentration that hair instrument is concentrated into cellulose solution is 7g/L, then by the fiber after concentration under 8000r/min high shear
The dilution heat of sulfuric acid that plain solution is 4% with mass fraction is 1 by volume:6 mixing, form mixed liquor；Finally by the mixed liquor
High-temperature acid hydrolyzes 1h under the conditions of 120 DEG C, makes cellulose monose, that is, obtains cellulose fermentable sugars.
Embodiment 3：The preparation of cellulose fermentable sugars
(1) take 7g known fibers element and hemicellulose level be respectively 95.33% and 1.73% over dry jute pulp and hydrogen-oxygen
It is 1 in mass ratio to change sodium and urea mixed solution:60 mixing, stirring, form uniform mixed system；Wherein, in mixed system
The mass fraction of sodium hydroxide and urea is respectively 9% and 11%.
(2) by mixed system under sealed conditions (system be fully sealed be in order to avoid the carbon dioxide in air with
Sodium hydroxide reacts) -10 DEG C are cooled to, and 7min is stirred under conditions of 8000r/min, obtain cellulose solution.
(3) hydrochloric acid solution for taking cellulose solution to be first 8mol/L with molar concentration adjusts PH to neutrality, then rotated steaming
The concentration that hair instrument is concentrated into cellulose solution is 8g/L, then by the fiber after concentration under 9000r/min high shear
The dilution heat of sulfuric acid that plain solution is 4% with mass fraction is 1 by volume:8 mixing, form mixed liquor；Finally by the mixed liquor
High-temperature acid hydrolyzes 1h under the conditions of 120 DEG C, makes cellulose monose, that is, obtains cellulose fermentable sugars.
Embodiment 4：The preparation of cellulose fermentable sugars
(1) take 7g known fibers element and hemicellulose level be respectively 95.33% and 1.73% over dry jute pulp and hydrogen-oxygen
It is 1 in mass ratio to change sodium and urea mixed solution:60 mixing, stirring, form uniform mixed system；Wherein, in mixed system
The mass fraction of sodium hydroxide water and urea is respectively 10% and 15%.
(2) by mixed system under sealed conditions (system be fully sealed be in order to avoid the carbon dioxide in air with
Sodium hydroxide reacts) -12 DEG C are cooled to, and 10min is stirred under conditions of 9000r/min, obtain cellulose solution.
(3) hydrochloric acid solution for taking cellulose solution to be first 6mol/L with molar concentration adjusts PH to neutrality, then rotated steaming
The concentration that hair instrument is concentrated into cellulose solution is 10g/L, then by the fiber after concentration under 9000r/min high shear
The dilution heat of sulfuric acid that plain solution is 4% with mass fraction is 1 by volume:12 mixing, form mixed liquor；Finally by the mixed liquor
High-temperature acid hydrolyzes 1h under the conditions of 120 DEG C, makes cellulose monose, that is, obtains cellulose fermentable sugars.
Effect example
The cellulose solution of the monose obtained in above-described embodiment 1~4 is surveyed to the concentration of each monose, measuring method is：
First with 1mol/L sodium hydroxide solution and H therein+, then with distilled water diluting certain multiple (avoid monose in solution
Concentration is too high, and data measured is inaccurate), finally measure glucose in solutions, xylose and mannose with high performance liquid chromatography
Concentration.The concentration of glucose, xylose and mannose need to use the multiple for measuring numerical value and being multiplied by dilution in original solution, as a result such as the institute of table 1
Show.
The concentration of glucose, xylose and mannose in the original solution of table 1
Note：Ideally, 1kg pure cellulose or poly- mannose can hydrolyze to obtain 1.111kg corresponding monose,
1kg xylan can hydrolyze to obtain 1.111kg corresponding monose.
As it can be seen from table 1 the acid saccharification efficiency maximum of the cellulose obtained using this preparation method is reachable
86.99%, the acid saccharification efficiency of hemicellulose is maximum up to 98.95%, has higher saccharification efficiency.And in whole process
The chemicals used is cheap and smaller to the contaminative of environment and equipment.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of cellulose fermentable sugars, it is characterised in that comprise the following steps：
(1) it is 1 in mass ratio by jute pulp and sodium hydroxide/urea mixed solution：Stirred after 40~60 mixing, obtain mixture
System；
(2) mixed system obtained in step (1) is cooled to -8~-12 DEG C, stirring and dissolving, obtains cellulose solution；
(3) by step (2) cellulose solution carry out neutralisation treatment, concentration, then by the cellulose solution after concentration with it is dilute
Sulfuric acid solution is 1 by volume：4~12 mixing, then sour water solution is carried out, obtain cellulose fermentable sugars.
2. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
The mass fraction 5~10% of sodium hydroxide in mixed system described in step (1), the mass fraction 3~15% of urea；
The concentration of dilution heat of sulfuric acid described in step (3) is mass percent 4%.
3. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
The speed of stirring described in step (2) is 3000~9000r/min；
Addition dilution heat of sulfuric acid described in step (3) is dilute to be slowly added under 6000~9000r/min high shear
Sulfuric acid solution.
4. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
Acid described in step (3) is hydrolyzed to hydrolyzes 1h under the conditions of 120 DEG C.
5. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
Neutralisation treatment described in step (3) is to adjust PH to neutrality using hydrochloric acid solution；The molar concentration of described hydrochloric acid solution
For 5~8mol/L.
6. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
Concentration described in step (3) is to use Rotary Evaporators that cellulose solution is concentrated into concentration for 6~10g/L.
7. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
Jute pulp described in step (1) is known fiber element and the over dry jute pulp of hemicellulose level.
8. the preparation method of cellulose fermentable sugars according to claim 1, it is characterised in that：
It is cooled to carry out under air-proof condition described in step (2)；
The time of stirring described in step (2) is 5~10min.
A kind of 9. cellulose fermentable sugars, it is characterised in that：It is prepared by the method described in any one of claim 1~8.
10. application of the cellulose fermentable sugars in bio-ethanol field described in claim 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101160409A (en) * | 2005-04-12 | 2008-04-09 | 纳幕尔杜邦公司 | System and process for biomass treatment |
| CN101628920A (en) * | 2009-08-17 | 2010-01-20 | 福州大学 | Comprehensive utilization method of corn cob |
| CN101725068A (en) * | 2008-10-29 | 2010-06-09 | 三星电子株式会社 | Method and device for fractionizing a biomass based on lignocellulose |
| CN102690897A (en) * | 2012-05-22 | 2012-09-26 | 中国科学院宁波材料技术与工程研究所 | Two-step hydrolysis method for preparing reducing sugars with cellulose |
| CN105755071A (en) * | 2016-04-01 | 2016-07-13 | 江苏大学 | Method for preparing fermentable sugar or bioethanol by utilizing biomass and 'one-pot method' |
-
2017
- 2017-08-01 CN CN201710645675.5A patent/CN107501357A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101160409A (en) * | 2005-04-12 | 2008-04-09 | 纳幕尔杜邦公司 | System and process for biomass treatment |
| CN101725068A (en) * | 2008-10-29 | 2010-06-09 | 三星电子株式会社 | Method and device for fractionizing a biomass based on lignocellulose |
| CN101628920A (en) * | 2009-08-17 | 2010-01-20 | 福州大学 | Comprehensive utilization method of corn cob |
| CN102690897A (en) * | 2012-05-22 | 2012-09-26 | 中国科学院宁波材料技术与工程研究所 | Two-step hydrolysis method for preparing reducing sugars with cellulose |
| CN105755071A (en) * | 2016-04-01 | 2016-07-13 | 江苏大学 | Method for preparing fermentable sugar or bioethanol by utilizing biomass and 'one-pot method' |
Non-Patent Citations (1)
| Title |
|---|
| 张美云: "《造纸技术》", 31 January 2014, 中国轻工业出版社 * |
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