CN108842008A - A kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution - Google Patents
A kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution Download PDFInfo
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- CN108842008A CN108842008A CN201810757853.8A CN201810757853A CN108842008A CN 108842008 A CN108842008 A CN 108842008A CN 201810757853 A CN201810757853 A CN 201810757853A CN 108842008 A CN108842008 A CN 108842008A
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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Abstract
The present invention relates to a kind of methods that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution.Include the following steps：(1) it is acidified：Acid solution is added into slurrying pre-hydrolyzed solution, is acidified pre-hydrolyzed solution；(2) hydro-thermal acidolysis：Pre-hydrolyzed solution obtained by step (1) is adjusted to hydrothermal temperature, makes pre-hydrolyzed solution that hydro-thermal acidolysis reaction occur and prepares xylo-oligosaccharide solution.The present invention prepares xylo-oligosaccharide solution using papermaking enterprise slurrying pre-hydrolyzed solution as raw materials for production, using hydro-thermal acid hydrolyzation processing slurrying pre-hydrolyzed solution, and preparation process is simple, time-consuming short, production cost is low, and product added value is high, it is convenient for industrialized production, can be widely applied to the papermaking enterprise of production dissolving pulp.
Description
Technical field
The present invention relates to a kind of methods that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution, belong to chemical industry, food
Product technical field.
Background technique
Xylo-oligosaccharide is as 2~7 xylose molecules with oligosaccharide made of β-Isosorbide-5-Nitrae glucosides key connection.Xylo-oligosaccharide is heat-resisting,
It is acidproof, there is the proliferation for promoting the beneficial bacteriums such as Bifidobacterium in human body, improve human gastrointestinal tract, promote body cell health, increase
Strong immunity of organisms, anti-caries promote human body to healthcare functions such as the absorptions of calcium, are to be widely used in food, drug and makeup
The important functional oligose of one kind of the industry such as product.Xylo-oligosaccharide and other function oligosaccharide (for example, soyabean oligosaccharides,
Oligofructose and oligoisomaltose etc.) it compares, have the characteristics that easy to use, safe, stable, economic value is high.
Currently, being mainly enzymatic hydrolysis, Acid hydrolysis and Zi Shui by the method for hydrolysis that hemicellulose degradation is xylo-oligosaccharide
Three kinds of solution.Wherein because enzymatic hydrolysis reaction condition is mild and gained liquid glucose in impurity it is few due to become and prepare the master of xylo-oligosaccharide
Want method.However, enzymatic hydrolysis production xylo-oligosaccharide also exposes many disadvantages in the industrial production, for example, in reaction process
Condition, which is difficult to control, causes enzyme to inactivate, and the production cost increases, and the binding site deficiency of enzyme and sugar causes xylo-oligosaccharide yield lower
Deng.Acid system degradation is more thorough, is relatively low cost and easy to operate, but the key of reaction time, temperature, acid concentration as degradation
Factor, condition too acutely be easy to cause most of xylan degrading for the wooden monosaccharide.Therefore, suitable acid hydrolysis conditions are explored
It is most important for efficiently producing xylo-oligosaccharide.
During slurrying enterprise prepares paper pulp, needing will be big in lignocellulose raw material by the prehydrolysis of high temperature hydro-thermal
The removal of part hemicellulose.Cellulose is mainly contained in the solid matter that prehydrolysis obtains, for further preparing paper pulp.So
And the liquid phase that prehydrolysis obtains is burned off in chemical recovery system, causes the wave of a large amount of hemicellulose resources in pre-hydrolyzed solution
Take.Since xylan content accounts for 80% or more of total sugar content in pre-hydrolyzed solution in slurrying pre-hydrolyzed solution, with papermaking enterprise
Slurrying pre-hydrolyzed solution is raw materials for production, prepares xylo-oligosaccharide solution using hydro-thermal acid hydrolyzation processing slurrying pre-hydrolyzed solution, prepares work
Skill is simple, and production cost is low, and product added value is high.
Summary of the invention
Present invention aim to address the Rational Utilizations of above-mentioned slurrying pre-hydrolyzed solution, provide a kind of slurrying pre-hydrolyzed solution
The method that hydro-thermal acidolysis prepares xylo-oligosaccharide solution.Keep the xylan in slurrying pre-hydrolyzed solution efficient by the method for hydro-thermal acidolysis
Ground is degraded to xylo-oligosaccharide.Xylan therein is effectively degraded to using the feature for being rich in hemicellulose in slurrying pre-hydrolyzed solution
Xylo-oligosaccharide, to realize that the increment of pre-hydrolyzed solution utilizes.
The technical solution adopted by the present invention is as follows：
A kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution, includes the following steps：
(1) it is acidified：Acid solution is added into slurrying pre-hydrolyzed solution, is acidified pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：Pre-hydrolyzed solution obtained by step (1) is adjusted to hydrothermal temperature, makes pre-hydrolyzed solution that water occur
Hot acidolysis reaction prepares xylo-oligosaccharide solution.
Acid solution in the step (1) includes organic acid soln and inorganic acid solution, and wherein organic acid soln includes
The solution such as formic acid, acetic acid, inorganic acid solution include the solution such as sulfuric acid, hydrochloric acid, nitric acid.The additional amount of acid solution is the pre- water of slurrying
Solve 0.1%~3% (in terms of water-free solution) of liquid mass fraction.
Hydro-thermal acidolysis temperature in the step (2) is 100~180 degrees Celsius, and the reaction time is 0~3.5 hour.With it is existing
There is technology to compare, beneficial effects of the present invention：
(1) present invention prepares xylo-oligosaccharide solution using hydro-thermal acid hydrolyzation processing slurrying pre-hydrolyzed solution, and preparation process is simple,
Time-consuming short, production cost is low, is convenient for industrialized production.
(2) present invention prepares xylo-oligosaccharide solution, product added value by raw materials for production of papermaking enterprise slurrying pre-hydrolyzed solution
Height solves the problems, such as the processing of slurrying pre-hydrolyzed solution, with good economic efficiency.
Specific embodiment
Below with reference to embodiment, invention is described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the sulfuric acid of addition 0.1% is (with water-free
Sulphur acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 120 degrees Celsius, is reacted 1.0 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 2
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the hydrochloric acid of addition 0.3% is (with water-free
Hydrochloric acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 105 degrees Celsius, is reacted 2.0 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 3
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the nitric acid of addition 1.0% is (with water-free
Nitric acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 120 degrees Celsius, is reacted 1.5 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 4
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the phosphoric acid of addition 3.0% is (with water-free
Phosphoric acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 135 degrees Celsius, is reacted 0 hour；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 5
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the hydrochloric acid of addition 0.2% is (with water-free
Hydrochloric acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 100 degrees Celsius, is reacted 3.0 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 6
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the sulfuric acid of addition 0.8% is (with water-free
Sulphur acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 150 degrees Celsius, is reacted 2.5 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 7
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the nitric acid of addition 0.1% is (with water-free
Nitric acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 180 degrees Celsius, is reacted 3.5 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
Embodiment 8
(1) it is acidified：Into the reaction vessel for filling 50mL slurrying pre-hydrolyzed solution, the sulfuric acid of addition 0.3% is (with water-free
Sulphur acid meter), it stirs evenly, is acidified slurrying pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：The slurrying pre-hydrolyzed solution being acidified in step (1) is warming up to 120 degrees Celsius, is reacted 2.0 hours；
(3) the xylo-oligosaccharide yield for testing the present embodiment is listed in table 1.
The xylo-oligosaccharide yield of slurrying pre-hydrolyzed solution in 1 Examples 1 to 8 of table.
| Xylo-oligosaccharide yield/g/L | |
| Embodiment 1 | 7.23 |
| Embodiment 2 | 8.25 |
| Embodiment 3 | 6.04 |
| Embodiment 4 | 6.84 |
| Embodiment 5 | 8.82 |
| Embodiment 6 | Trace |
| Embodiment 7 | Trace |
| Embodiment 8 | 11.63 |
Claims (4)
1. a kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution, which is characterized in that include the following steps：
(1) it is acidified：Acid solution is added into slurrying pre-hydrolyzed solution, is acidified pre-hydrolyzed solution；
(2) hydro-thermal acidolysis：Pre-hydrolyzed solution obtained by step (1) is adjusted to hydrothermal temperature, makes pre-hydrolyzed solution that hydro-thermal acid occur
Solution reaction prepares xylo-oligosaccharide solution.
2. a kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution according to claim 1, special
Sign is that the slurrying pre-hydrolyzed solution includes gained pre-hydrolyzed solution and other chemistry in prehydrolytic sulfate process pulping process
Starch gained pre-hydrolyzed solution in preparation process.
3. a kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution according to claim 1, special
Sign is that acid solution described in step (1) includes organic acid soln and inorganic acid solution, and wherein organic acid soln includes first
The solution such as acid, acetic acid, inorganic acid solution include the solution such as sulfuric acid, hydrochloric acid, nitric acid.The additional amount of acid solution is slurrying prehydrolysis
0.1%~3% (in terms of water-free solution) of liquid mass fraction.
4. a kind of method that the hydro-thermal acidolysis of slurrying pre-hydrolyzed solution prepares xylo-oligosaccharide solution according to claim 1, special
Sign is that hydro-thermal acidolysis temperature described in step (2) is 100~180 degrees Celsius, and the reaction time is 0~3.5 hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823263A (en) * | 2018-07-11 | 2018-11-16 | 北京林业大学 | A kind of method of slurrying pre-hydrolyzed solution preparation of xylooligosaccharideswith with enzyme solution |
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| CN103740787A (en) * | 2014-01-17 | 2014-04-23 | 山东大学 | Method for producing xylooligosaccharide by use of broadleaf wood dissolving pulp prehydrolysis waste liquid enzyme process |
| CN104988783A (en) * | 2015-07-23 | 2015-10-21 | 长沙理工大学 | Pulping method of reed organic solvent slurry by pre-extracting hemicellulose and product thereof |
| CN106755615A (en) * | 2016-12-07 | 2017-05-31 | 南京工业大学 | Method for preparing xylo-oligosaccharide by jointly degrading lignocellulose biomass through hydrothermal method and dilute acetic acid hydrolysis method |
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| CN103740787A (en) * | 2014-01-17 | 2014-04-23 | 山东大学 | Method for producing xylooligosaccharide by use of broadleaf wood dissolving pulp prehydrolysis waste liquid enzyme process |
| CN104988783A (en) * | 2015-07-23 | 2015-10-21 | 长沙理工大学 | Pulping method of reed organic solvent slurry by pre-extracting hemicellulose and product thereof |
| CN106755615A (en) * | 2016-12-07 | 2017-05-31 | 南京工业大学 | Method for preparing xylo-oligosaccharide by jointly degrading lignocellulose biomass through hydrothermal method and dilute acetic acid hydrolysis method |
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| CN108823263A (en) * | 2018-07-11 | 2018-11-16 | 北京林业大学 | A kind of method of slurrying pre-hydrolyzed solution preparation of xylooligosaccharideswith with enzyme solution |
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