CN106834554A - A kind of method that hemicellulose continuous hydrolysis prepare xylose - Google Patents
A kind of method that hemicellulose continuous hydrolysis prepare xylose Download PDFInfo
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- CN106834554A CN106834554A CN201710116872.8A CN201710116872A CN106834554A CN 106834554 A CN106834554 A CN 106834554A CN 201710116872 A CN201710116872 A CN 201710116872A CN 106834554 A CN106834554 A CN 106834554A
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- hemicellulose
- xylose
- acid
- tubular reactor
- continuous hydrolysis
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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 invention belongs to xylose production field, the method that specially a kind of hemicellulose continuous hydrolysis prepare xylose.The method is comprised the following steps：Take the material containing hemicellulose to be crushed, then enter in nanometer emulsified machine simultaneously with water, be continuously made into aqueous emulsion, then continuously entering high-shear emulsion machine with acidic catalyst again is emulsified, and makes stable emulsion.Continous way tubular reactor being squeezed into pump to be hydrolyzed, obtaining xylose hydrolysis fluid, conversion ratio is up to 85 95%.Wherein unreacted hemicellulose, precipitation is reinstated centrifuge and is separated with solid acid one, returns to emulsification process.Cleaner liquid is if sulfuric acid or hydrochloric acid should then be neutralized；Obtain the aqueous solution containing xylose 5 12%；Can be directly used for preparing furfural.Or removal of impurities, decolouring, desalination, concentration, crystallization are carried out with existing film process patented technology obtain refined xylose.The sufficient raw of this method, preparation process serialization, automates, reaches efficiently production, and xylose rate is high.
Description
Technical field
The invention belongs to xylose production field, the method that specially a kind of hemicellulose continuous hydrolysis prepare xylose.
Background technology
Xylose is a kind of naturally occurring pentose, is present in plant with polycondensation state.Finished product xylose be white crystals or
Crystalline powder, it is soluble in water.Xylose does not have energy value with absorption is not digested；Bifidobacterium Bifidum in activating human body enteron aisle
And promote its growth；Do not utilized by Institute of Micro-biology in oral cavity, possess the part physiological function of dietary fiber, it is possible to decrease serum cholesterol
Prevention intestinal cancer etc.；Xylose is taken in simultaneously with calcium, can improve absorptivity and retention rate of the human body to calcium；Constipation etc. can be prevented many
Plant physiological function.Xylose is widely used in manufacture xylitol；Food, beverage；Feed for pet；Baked goods；High-grade color of soy sauce；Gently
The aspects such as work, chemical industry.The xylitol for especially being manufactured as raw material with xylose, because of its sugar-free, possesses the mouthfeel similar with sucrose and sweet
Degree, blood glucose value is not influenceed, can be widely used by many physiological functions such as diabetes, bariatric patients are edible.It is wooden at present
Sugared is mainly raw material with agricultural wastes such as the corncob rich in pentosan, bagasse, and corncob and bagasse are xylose lifes
The primary raw material of product, cellulose is 32%-48%, hemicellulose 24%~25%, lignin 18%-20%, ash in its composition
Divide about 4%.Through hydrolysis, neutralize, decolourize, refined purification, concentration, crystallization, separate, the operation such as drying is obtained.But with plant material
Production xylose, operation is more, seriously polluted, high cost, be also subject to seasonal restrictions sometimes.
In the production process of with chemical fiber pulp as raw material (wood pulp, cotton pulp, bamboo pulp) production viscose rayon, due to containing in raw material
There is more hemicellulose, it is necessary to the hemicellulose in raw material is removed；Then its dissolution is filtered with membrane technology with alkali lye generally
Go out alkali lye reuse, and hemicellulose does not have good utilization ways.Produced with the hemicellulose of viscose rayon production devil liquor recovery
Xylose, there is not yet report.
The content of the invention
The present invention is based on above technical problem, there is provided a kind of sufficient raw, preparation process serialization, automatic
Change, can reach the method that the hemicellulose continuous hydrolysis of efficiently production purpose prepare xylose.
The technical scheme is that：
A kind of method that hemicellulose continuous hydrolysis prepare xylose, the method is comprised the following steps：
1) material containing hemicellulose is taken, the aqueous emulsion of the concentration of 6-15wt% containing hemicellulose is made into.The hemicellulose thing
Expect that the hemicellulose level reclaimed from chemical fibre waste fluid is 8- for the solid hemicellulose or hemicellulose level of 70-80%
12% liquid, if with liquid, emulsion process can be saved.If solid hemicellulose, then need to be crushed to 1-5nm with pulverizer,
Entered in nanometer emulsified machine simultaneously with the flow of the flow of 6-15Kg/h and water 94-85Kg/h, be continuously made into 6- containing hemicellulose
The aqueous emulsion of 15% concentration.
2) (in terms of the addition quality of reaction solution, sulfuric acid is 3-5%, hydrochloric acid 4-6% or solid acid 3- to same acidic catalyst
6%), continuously enter high-shear emulsion machine and emulsify and make the stable emulsion containing hemicellulose 6-15%.Beaten with pump
Enter continous way tubular reactor, tubular reactor temperature control is hydrolyzed at 70-130 DEG C；Reactant is in tubular reactor
The middle residence time is 20-60 minutes, obtains xylose hydrolysis fluid, and then conversion ratio is separated with centrifuge again up to 85-95%, essence
Xylose is obtained.If when making acidic catalyst using sulfuric acid or hydrochloric acid, then the clear liquid that centrifuge is separated is tackled, after being neutralized
With the desalination of existing film patented technology, the aqueous solution containing xylose 5-12% is concentrated to give, the aqueous solution can be directly used for preparing chaff
Aldehyde；Or removal of impurities, decolouring, desalination, concentration, crystallization are carried out with existing film process patented technology obtain refined xylose.If
When making acidic catalyst using solid acid, wherein unreacted hemicellulose, analyses due to destroying emulsification condition in reaction
Go out to reinstate centrifuge with solid acid one and separate, return to emulsification process.
, selected from any one or more in basic zirconium phosphate, phosphoric acid tin, solid heteropoly acid, addition is with anti-for described solid acid
The weight/mass percentage composition of solution is answered to be calculated as 3-6%.
Mulser can select the one kind in high-shear emulsion machine, solid-liquid mulser, nanometer emulsified machine.
Tubular reactor pipe is mixed built with SV type static mixer annexes with the liquid liquid for ensuring immiscible
Uniformly, according to the requirement of residence time, promote reaction complete, tubular reactor length is 20-25m, now between each reaction tube
Can be interconnected with 180 ° of elbow, component units reactor.There are steam heating jacket, control reaction outside tubular reactor
Temperature is at 70-130 DEG C.By PLC control modules in production process, it is connected with pump and reactor respectively, controls flow and reactor
Temperature.
% in present specification, unless otherwise specified, represents its weight/mass percentage composition.
Compared with prior art, beneficial effects of the present invention are：
(1), sufficient raw,
(2), using nanometer emulsified machine, material liquid is well mixed with catalyst, be conducive to the carrying out of reaction.
(3) preparation process serialization, automate, reach efficiently production, xylose rate is high.
Brief description of the drawings：
Fig. 1 is the process flow diagram using inorganic acid catalyst described in the embodiment of the present invention 1.
Fig. 2 is the process flow diagram using solid acid catalyst described in the embodiment of the present invention 2.
Specific embodiment
In order that present disclosure easily facilitates understanding, below in conjunction with the drawings and specific embodiments in the present invention
Described technique is further elaborated.But this scope for being interpreted as above-mentioned theme of the invention should not be only limitted to following implementations
Example.
Embodiment 1：
In terms of weight/mass percentage composition, the solid hemicellulose of content 70% is taken, 1-5nm is crushed to pulverizer, with 17Kg/
The flow of h enters in nanometer emulsified machine simultaneously with the flow of water 83Kg/h, is continuously made into the water and milk containing the concentration of hemicellulose 12%
Liquid, then again with the flow of acidic catalyst hydrochloric acid 5Kg/h, continuously enters high-shear emulsion machine and carries out emulsification and make containing half
The stable emulsion of cellulose 12%.Continous way tubular reactor is squeezed into pump, tubular reactor temperature control is entered at 120 DEG C
Water-filling solution；The residence time is 25 minutes to reactant in a tubular reactor, obtains xylose hydrolysis fluid, and conversion ratio is up to 94%.Its
In unreacted hemicellulose, separated out due to destroying emulsification condition in reaction, separated with centrifuge, return to emulsification work
Sequence.The clear liquid that centrifuge is separated, after being neutralized with NaOH with the desalination of existing film patented technology, be concentrated to give and obtain containing xylose
The aqueous solution of 10wt%；Xylose rate is up to 94%.Can be directly used for preparing furfural.Or with existing film process patented technology
Carry out removal of impurities, decolouring, desalination, concentration, crystallization and obtain refined xylose.
Tubular reactor pipe is mixed built with SV type static mixer annexes with the liquid liquid for ensuring immiscible
Uniformly, according to the requirement of residence time, promote reaction complete, tubular reactor length is 16m, can now be used between each reaction tube
180 ° of elbow is interconnected, component units reactors.There are steam heating jacket, controlling reaction temperature outside tubular reactor
At 120 DEG C.By PLC control modules in production process, it is connected with pump and reactor respectively, controls flow and temperature of reactor.This
The continuous hydrolysis of invention hydrolyze the influence to conversion ratio with batch tank, see the table below：
| Hydrolysis residence time min | Xylose yield % | |
| Batch still is hydrolyzed | 90 | 85 |
| Continuous hydrolysis of the present invention | 30 | 94 |
Embodiment 2：
In terms of weight/mass percentage composition, the solid hemicellulose of content 70% is taken, 1-5nm is crushed to pulverizer, with 14Kg/
The flow of h enters in nanometer emulsified machine simultaneously with the flow of water 86Kg/h, is continuously made into the water and milk containing the concentration of hemicellulose 10%
Liquid, then again with the flow of solid acid catalyst heteropoly acid 4Kg/h, continuously enters high-shear emulsion machine and carries out emulsification and be allowed into
It is the stable emulsion containing hemicellulose 12%.Continous way tubular reactor is squeezed into pump, tubular reactor temperature control is 120
It is hydrolyzed at DEG C；The residence time is 30 minutes to reactant in a tubular reactor, obtains xylose hydrolysis fluid, special with existing film
Sharp technology desalination, it is concentrated to give the aqueous solution obtained containing xylose 10wt%；Conversion ratio is up to 90%.Wherein unreacted half is fine
Dimension element, separates out due to destroying emulsification condition in reaction and reinstate centrifuge with solid acid one and separates, return emulsification process.Obtain
The aqueous solution containing xylose 10wt%；Can be directly used for preparing furfural.Or removal of impurities is carried out with existing film process patented technology, is taken off
Color, desalination, concentration, crystallization obtain refined xylose.
Tubular reactor pipe is mixed built with SV type static mixer annexes with the liquid liquid for ensuring immiscible
Uniformly, according to the requirement of residence time, promote reaction complete, tubular reactor length is 20m, can now be used between each reaction tube
180 ° of elbow is interconnected, component units reactors.There are steam heating jacket, controlling reaction temperature outside tubular reactor
At 120 DEG C.By PLC control modules in production process, it is connected with pump and reactor respectively, controls flow and temperature of reactor.It is real
Apply example 3,
In terms of weight/mass percentage composition, the hemicellulose aqueous solution of content 10% is taken, with the flow of 100Kg/h, urged with acidity
The flow of agent sulfuric acid 3Kg/h, continuously enters high-shear emulsion machine and emulsify and make the stabilization containing hemicellulose 10%
Emulsion.Continous way tubular reactor is squeezed into pump, tubular reactor temperature control is hydrolyzed at 110 DEG C；Reactant exists
The residence time is 30 minutes in tubular reactor, obtains xylose hydrolysis fluid, and conversion ratio is up to 92%.Wherein unreacted half is fine
Dimension element, due to destroying emulsification condition in reaction and precipitation centrifuge is separated, returns to emulsification process.It is clear that centrifuge is separated
Liquid, after being neutralized with NaOH with the desalination of existing film patented technology, be concentrated to give the aqueous solution that obtains containing xylose 9wt%；Can
It is directly used in and prepares furfural.Or removal of impurities, decolouring, desalination, concentration, crystallization are carried out with existing film process patented technology obtain essence
Xylose processed.
Tubular reactor pipe is mixed built with SV type static mixer annexes with the liquid liquid for ensuring immiscible
Uniformly, according to the requirement of residence time, promote reaction complete, tubular reactor length is 16m, can now be used between each reaction tube
180 ° of elbow is interconnected, component units reactors.There are steam heating jacket, controlling reaction temperature outside tubular reactor
At 120 DEG C.By PLC control modules in production process, it is connected with pump and reactor respectively, controls flow and temperature of reactor.
Although the present invention has passed through specific embodiment being elaborated to it, this professional ordinary skill
Personnel should be understood that any form without departing from claims and the change of details made on this basis,
Belong to invention which is intended to be protected.
Claims (7)
1. a kind of method that hemicellulose continuous hydrolysis prepare xylose, it is characterised in that comprise the following steps：
1）The material containing hemicellulose is taken, the aqueous emulsion of the concentration of 6-15wt% containing hemicellulose is made into；
2）Then same acidic catalyst again, continuously enters mulser and emulsify and make the stabilization containing hemicellulose 6-15%
Emulsion；
3）By step 2）In stable emulsion pump squeeze into continous way tubular reactor, tubular reactor temperature control is in 70-
It is hydrolyzed at 130 DEG C；The residence time is 20-60 minutes to reactant in a tubular reactor, obtains xylose hydrolysis fluid, then with from
Scheming is separated, and is refining to obtain xylose.
2. a kind of method that hemicellulose continuous hydrolysis prepare xylose according to claim 1, it is characterised in that：Described half
The solid hemicellulose or hemicellulose level that cellulose substances are reclaimed from chemical fibre waste fluid are the liquid of 8-12wt%.
3. according to claim 1 a kind of hemicellulose continuous hydrolysis prepare xylose method it is characterized in that：Described acid
Property catalyst be sulfuric acid 3-5%, hydrochloric acid 4-6% or solid acid 3-6%, wherein to be selected from basic zirconium phosphate, phosphoric acid tin, solid miscellaneous more for solid acid
The mixture of any one or more in acid.
4. a kind of method that hemicellulose continuous hydrolysis prepare xylose according to claim 3, it is characterised in that：When step 2）
In acid catalyst used when being sulfuric acid or hydrochloric acid, after it is separated with centrifuge, the clear liquid that will be obtained neutralized after with existing
Membrane technology obtains the aqueous solution containing xylose 5-12wt% after carrying out desalination, concentration；When step 2）In acid catalyst used be
During solid acid, by step 3）Still unreacted hemicellulose, separates out due to destroying emulsification condition in reaction afterwards, and solid
Centrifuge separation is reinstated in acid one, returns to emulsification process.
5. a kind of method that hemicellulose continuous hydrolysis prepare xylose according to claim 1, it is characterised in that：Described breast
Change machine is from any one in high-shear emulsion machine, solid-liquid mulser, nanometer emulsified machine.
6. a kind of method that hemicellulose continuous hydrolysis prepare xylose according to claim 1, it is characterised in that：Described pipe
Formula reactor tube built with SV type static mixer annexes, to ensure that immiscible liquid liquid is mixed uniformly, according to stopping
The requirement of time is stayed, promotes that reaction is complete, tubular reactor length is 20-25m, now with 180 ° of elbow between each reaction tube
To interconnect, component units reactor.
7. a kind of method that hemicellulose continuous hydrolysis prepare xylose according to claim 1, it is characterised in that：Tubular reactor
Steam heating jacket is provided with outside device, controlling reaction temperature is at 70-130 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710116872.8A CN106834554A (en) | 2017-03-01 | 2017-03-01 | A kind of method that hemicellulose continuous hydrolysis prepare xylose |
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| CN201710116872.8A CN106834554A (en) | 2017-03-01 | 2017-03-01 | A kind of method that hemicellulose continuous hydrolysis prepare xylose |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
| CN109355443A (en) * | 2018-12-04 | 2019-02-19 | 浙江华康药业股份有限公司 | A kind of hemicellulose continuous hydrolysis prepares the system and method for Xylose |
| CN110128488A (en) * | 2019-04-28 | 2019-08-16 | 宁波兴隆巨创机电科技有限公司 | A kind of preprocess method and its system of the lignocellulosic based on xylo-oligosaccharide preparation |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
| CN107475467B (en) * | 2017-09-14 | 2020-12-22 | 齐鲁工业大学 | Efficient extraction method of poplar xylose |
| CN109355443A (en) * | 2018-12-04 | 2019-02-19 | 浙江华康药业股份有限公司 | A kind of hemicellulose continuous hydrolysis prepares the system and method for Xylose |
| CN109355443B (en) * | 2018-12-04 | 2020-07-17 | 浙江华康药业股份有限公司 | System and method for preparing xylose liquid by continuous hydrolysis of hemicellulose |
| US12060621B2 (en) | 2018-12-04 | 2024-08-13 | Zhejiang Huakang Pharmaceutical Co., Ltd. | System for preparing xylose liquid by continuously hydrolyzing hemicellulose and method thereof |
| CN110128488A (en) * | 2019-04-28 | 2019-08-16 | 宁波兴隆巨创机电科技有限公司 | A kind of preprocess method and its system of the lignocellulosic based on xylo-oligosaccharide preparation |
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