CN105876168B - A kind of plant material controlled hydrolysis produces compound and functional oligose feed addictive method - Google Patents
A kind of plant material controlled hydrolysis produces compound and functional oligose feed addictive method Download PDFInfo
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- CN105876168B CN105876168B CN201610347424.4A CN201610347424A CN105876168B CN 105876168 B CN105876168 B CN 105876168B CN 201610347424 A CN201610347424 A CN 201610347424A CN 105876168 B CN105876168 B CN 105876168B
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Abstract
The invention discloses a kind of plant material controlled hydrolysis to produce compound and functional oligose feed addictive method.In plant material reaction system, using 10%~20% acetic acid as catalyst, to destroy cell wall structure and generating functionality xylo-oligosaccharide is formed in 120~150 DEG C of 10~60min of processing, cellooligosaccharide and dietary fiber, it include the organic acids such as acetic acid and formic acid to 5%~10% calcium hydroxide or calcium oxide suspension being added into reaction system with rapid neutralize by online forced feed mode at the end of reaction, the pH value of reaction system is set quickly to be increased to 6.5~7.0, to efficiently inhibit, the degradation of acid catalyzed oligomerization xylose generates xylose and material further degrades and generates the reaction of the impurity such as furans；Acetic acid is converted into dystectic calcium acetate and calcium formate inorganic salts simultaneously, to prevent the volatilization loss of acetic acid during high temperature blowing.Using this method, yield of oligosaccharide is improved, and impurity content is reduced, and can be produced and be obtained compound and functional oligose feedstuff additive product.
Description
One, technical field
The present invention relates to biological product technical field, in particular to a kind of plant material controlled hydrolysis produces compound and function
The method of energy property oligosaccharide feed addictive.
Two, background technique
Xylo-oligosaccharide is to be proliferated best Bifidobacterium function, inhibition pathogen and corrupt substance growth in oligosaccharide, adjust
Intestinal flora balance promotes animal body to the optimal product of the mineral absorptions effect such as calcium, magnesium, phosphorus, is that one kind can increase place
The non-digestible feed addictive of main animal health.The production method of xylo-oligosaccharide mainly includes enzyme hydrolysis method, high temperature degradation method
And acid-hydrolysis method first has to the high endo-xylanase preparation for obtaining specificity, while needing precision wherein using enzyme hydrolysis method
Enzyme hydrolysis process is controlled, the enzymatic hydrolysis reaction time is generally longer.The resistance to pressure request of high temperature degradation method equipment is high, and by-product is more.Using
Common strong inorganic acid Hydrolyze method, cuts off glycosidic bond at random, may generate a large amount of furfurals and xylose, and corrosivity is high.It compares
For use acetic acid Catalytic processes mild condition, simple process, acetic acid is easily recycled, and production process is environmentally protective, production
It is at low cost, there is more wide application prospect.
It is that catalyst degradation plant material can effectively convert xylan generation xylo-oligosaccharide, while obtain part using acetic acid
Cellooligosaccharide simultaneously effectively destroys raw material natural structure generation dietary fiber (CN201410334306.0).Plant is catalyzed in acetic acid
In the reaction system of raw material, there is degradations to generate xylose and further degradation generation chaff aldehyde type impurities for the xylo-oligosaccharide of generation
Trend, while in raw material cellooligosaccharide and lignin etc. can also occur under high-temperature acidic hydrolysising condition degradation reaction generation
Complicated mortifier influences product quality.More importantly above-mentioned degradation reaction is generally that exothermic reaction will lead to material and exist
A large amount of acetic acid volatilization and loss are caused when high temperature blowing, form serious environmental pollution.
Three, summary of the invention
Goal of the invention: the deficiencies in the prior art are directed to, are passed through at the end of acetic acid catalysis plant material degradation reaction
Certain mass concentration calcium hydroxide or calcium oxide suspension is added into reaction system with rapid neutralize includes acetic acid and formic acid
Equal organic acids, make the pH value of reaction system quickly be increased to 6.5~7.0, thus efficiently inhibit under the high temperature conditions acid catalysis it is low
Xylan degradation generates xylose and material further degrades and generates the reaction of the impurity such as furans；Acetic acid is converted into height simultaneously
The calcium acetate and calcium formate inorganic salts of fusing point, to prevent the volatilization loss of acetic acid during high temperature blowing.It is rich to produce acquisition
Compound and functional oligose feed containing functional low polyxylose, cellooligosaccharide, dietary fiber, calcium acetate and calcium formate
Additive product.
Technical solution: in order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of plant material controlled hydrolysis produces compound and functional oligose feed addictive method, including following
Step:
It (1) is to urge with 10%~20% acetic acid (mass concentration) in the plant material reaction system rich in xylan
Agent is low with generating functionality xylo-oligosaccharide, fiber is formed to destroy cell wall structure in 120~150 DEG C of 10~60min of processing
Glycan and dietary fiber.To 5%~10% hydrogen-oxygen is added into reaction system by online forced feed mode at the end of reaction
Changing calcium or calcium oxide suspension (mass concentration) with rapid neutralize includes the organic acids such as acetic acid and formic acid, makes the pH of reaction system
Value is quickly increased to 6.5~7.0, so that acid catalyzed oligomerization xylose degradation under the high temperature conditions efficiently be inhibited to generate xylose and material
Further degradation generates the reaction of the impurity such as furfural class；Acetic acid is converted into dystectic calcium acetate simultaneously and calcium formate is inorganic
Salt, to prevent the volatilization loss of acetic acid during high temperature blowing；
(2) the xylo-oligosaccharide yield based on efficient liquid phase ion chromatography quantitative detection can be improved to the 45% of raw material xylan
More than, yield of fiber oligosaccharide can be improved to 6% or more of raw material glucan.Furfural and hydroxymethylfurfural class impurity contain in product
Amount reduces 50% or more, and the fixation retention rate of acetate in the feed is more than 98%.
In step (1), the plant material rich in xylan includes corncob, beech and stalk etc., the acetate concentration
For 10%~20% (mass concentration), 120~150 DEG C of reaction temperature, 10~60min of reaction time.
The neutralizer is the alkaline matter containing calcium ion, and is with calcium hydroxide or calcium oxide suspension
Preferably, the concentration that neutralizer is added is 5%~10% (mass concentration), and the pH value of reaction system is made quickly to be increased to 6.5~7.0.
The utility model has the advantages that dense by the way that certain mass is added into reaction system at the end of acetic acid catalysis plant material degradation reaction
Spending calcium hydroxide or calcium oxide suspension with rapid neutralize includes the organic acids such as acetic acid and formic acid, keeps the pH value of reaction system fast
Speed is increased to 6.5~7.0, so that acid catalyzed oligomerization xylose degradation under the high temperature conditions efficiently be inhibited to generate xylose and material into one
Step degradation generates the reaction of the impurity such as furans；Acetic acid is converted into dystectic calcium acetate and calcium formate inorganic salts simultaneously,
To prevent the volatilization loss of acetic acid during high temperature blowing.Compared with prior art, xylo-oligosaccharide yield can be significantly improved,
Shorten the reaction time simultaneously, reduces acetic acid loss, reduce environmental pollution, effectively improve whole productivity effect.And it can produce and obtain
Obtain the compound and functional oligose for being rich in functional low polyxylose, cellooligosaccharide, dietary fiber, calcium acetate and calcium formate
Feedstuff additive product.
Four, specific embodiment
Case study on implementation 1
In 15L mechanical agitation type stainless steel high-pressure reaction pot, 7L is added and contains 1kg plant material and 20% acetic acid (matter
Measure concentration) reactant, sealing controls speed of agitator 150r/min, is heated up to stop after 140 DEG C of heat preservation 30min heating, pass through
It includes acetic acid and first that 10% calcium hydroxide (mass concentration), which is added, into reaction system with rapid neutralize in online forced feed mode
The pH value of the organic acids such as acid, reaction system is quickly increased to 6.58, detects reaction solution ingredient using efficient liquid phase ion chromatography, instead
The yield for answering xylose in liquid, xylobiose, xylotriose, Xylotetrose, the wooden pentasaccharides, six sugar of wood, seven sugar of wood, Xylooctaose are respectively
34.93%, 15.00%, 11.98%, 11.54%, 5.74%, 4.40%, 2.60%, 1.63%, yield of fiber oligosaccharide is
The 6.72% of raw material glucan, furfural and hydroxymethylfurfural class impurity content, which less add calcium hydroxide, reduces 60.27%, vinegar
The fixation retention rate of acid group in the feed is 99.02%.
Case study on implementation 2
In 15L mechanical agitation type stainless steel high-pressure reaction pot, 10L is added and contains 2kg plant material and 10% acetic acid (matter
Measure concentration) reactant, sealing controls speed of agitator 160r/min, is heated up to stop after 130 DEG C of heat preservation 60min heating, pass through
It includes acetic acid and formic acid that 5% calcium hydroxide (mass concentration), which is added, into reaction system with rapid neutralize in online forced feed mode
Equal organic acids, the pH value of reaction system are quickly increased to 6.52, detect reaction solution ingredient, reaction using efficient liquid phase ion chromatography
Xylose in liquid, xylobiose, xylotriose, Xylotetrose, the wooden pentasaccharides, six sugar of wood, seven sugar of wood, Xylooctaose yield be respectively 24.54%,
12.04%, 10.87%, 11.46%, 6.29%, 5.25%, 4.21%, 2.78%, yield of fiber oligosaccharide is poly- for raw material Portugal
The 6.29% of sugar, furfural and hydroxymethylfurfural class impurity content less add calcium hydroxide and reduce 55.41%, and acetate is in original
Fixation retention rate in material is 98.78%.
Claims (2)
1. a kind of plant material controlled hydrolysis produces compound and functional oligose feed addictive method, feature exists
In, comprising the following steps:
(1) in the plant material reaction system rich in xylan, using the acetic acid of 10%~20% mass concentration as catalyst, In
120~150 DEG C of 10~60min of processing with destroy cell wall structure and form generating functionality xylo-oligosaccharide, cellooligosaccharide and
Dietary fiber；To at the end of reaction by online forced feed mode be added into reaction system calcium hydroxide or 5%~
10% mass concentration calcium oxide suspension neutralizes the organic acid including acetic acid and formic acid with rapid, keeps the pH value of reaction system quick
Be increased to 6.5~7.0, thus efficiently inhibit under the high temperature conditions acid catalyzed oligomerization xylose degradation generate xylose and material it is further
Degradation generates the reaction of chaff aldehyde type impurities；Acetic acid is converted into dystectic calcium acetate and calcium formate inorganic salts simultaneously, to prevent
Only during high temperature blowing acetic acid volatilization loss；
(2) the xylo-oligosaccharide yield based on efficient liquid phase ion chromatography quantitative detection can be improved to the 45% of raw material xylan with
On, yield of fiber oligosaccharide can be improved to 6% or more of raw material glucan；Furfural and hydroxymethylfurfural impurity content subtract in product
Few 50% or more, the fixation retention rate of acetate in the feed is more than 98%.
2. a kind of plant material controlled hydrolysis according to claim 1 produces compound and functional oligose feed addition
The method of agent, it is characterised in that: the plant material rich in xylan includes corncob, beech and stalk, the acetic acid quality
Concentration be 10%~20%, 120~150 DEG C of reaction temperature, 10~60min of reaction time.
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| CN110256510B (en) * | 2019-06-06 | 2023-03-07 | 南京林业大学 | Method for preparing multi-component xylo-oligosaccharide |
| CN113151614A (en) * | 2021-03-17 | 2021-07-23 | 南京林业大学 | Method for preparing xylooligosaccharide from agricultural and forestry waste through two-step acetic acid hydrolysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1759716A (en) * | 2004-10-15 | 2006-04-19 | 林翔云 | Method for joint producing oligo wood-spirit and calcium hydrogen phosphate in use for feedstuff |
| CN101089007A (en) * | 2006-06-16 | 2007-12-19 | 黄广民 | Process of preparing D-xylose and xyloligose with coconut shell |
| CN104164520A (en) * | 2014-07-15 | 2014-11-26 | 南京林业大学 | Method using acetic acid for controlled catalysis of orientational hydrolysis of xylan to prepare multicomponent xylooligosaccharide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1759716A (en) * | 2004-10-15 | 2006-04-19 | 林翔云 | Method for joint producing oligo wood-spirit and calcium hydrogen phosphate in use for feedstuff |
| CN101089007A (en) * | 2006-06-16 | 2007-12-19 | 黄广民 | Process of preparing D-xylose and xyloligose with coconut shell |
| CN104164520A (en) * | 2014-07-15 | 2014-11-26 | 南京林业大学 | Method using acetic acid for controlled catalysis of orientational hydrolysis of xylan to prepare multicomponent xylooligosaccharide |
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