CN101343292B - Continuous hydrolyzation method for cellulose series biomass and apparatus thereof - Google Patents
Continuous hydrolyzation method for cellulose series biomass and apparatus thereof Download PDFInfo
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- CN101343292B CN101343292B CN2008100302805A CN200810030280A CN101343292B CN 101343292 B CN101343292 B CN 101343292B CN 2008100302805 A CN2008100302805 A CN 2008100302805A CN 200810030280 A CN200810030280 A CN 200810030280A CN 101343292 B CN101343292 B CN 101343292B
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Abstract
The invention discloses a method for hydrolyzing cellulosic biomass continually, which is characterized in that solid biomass material mixed with water is conveyed into a horizontal type plug flow reactor, and a variable pitch spiral pushing rod is arranged inside the horizontal type plug flow reactor; at the same time, reaction solution is conveyed into the reactor, and the mixture is pushed by the variable pitch spiral pushing rod to advance so that the solid and the liquid are separated from each other; the solid residue is conveyed into a vertical countercurrent bed, then is conveyed upward by a constant pitch vertical spiral pushing rod, and at the same time is conveyed into the reaction solution from the upper part of a vertical countercurrent reactor; and finally, the solid residue is collected at the upper part of the vertical countercurrent reactor, and cellulosic hydrolysate is collected at the lower part of the vertical countercurrent reactor. The invention also comprises a device for realizing the method. The device comprises a continuous feeding air lock system, a horizontal type plug flow reactor and a vertical countercurrent reactor, wherein, a variable pitch spiral pushing rod is arranged inside the horizontal type plug flow reactor; the variable pitch spiral pushing rod comprises a feeding section, a principal reaction section and a pressing section; the feeding section is communicated with the continuous feeding air lock system; and the horizontal type plug flow reactor is communicated with the vertical countercurrent reactor by means of a residue conveying device.
Description
Technical field
The present invention relates to the biomass technical field, especially a kind of method of cellulose series biomass continuous hydrolysis and device.
Background technology
Along with energy dilemma and the environmental stress that the continuous consumption of a large amount of fossil fuel energies brings, the exploitation renewable energy source is subject to people's attention day by day.In numerous new forms of energy, biomass energy research has become the focus of renewable energy source research.Biomass are a kind of renewable and clean energy resource resources, produce alcohol fuel by lignocellulose biomass by hydrolyzation and come the instead of part fossil oil, alleviate one of effective ways of oil crisis.
Lignocellulose-like biomass is as the most promising fuel ethanol production raw material, and its production technique comprises that hydrolysis generates fermentable sugars, and sugar-fermenting is that ethanol and alcoholic acid dehydration are purified.Difficult point wherein is hydrolysis production fermentable sugars, and the method for lignocellulose biomass by hydrolyzation has acid hydrolysis and enzyme hydrolysis method, and extremely low acids hydrolysis method wherein comes into one's own day by day.
The research of acid hydrolytic reaction device has important pushing effect for the development and the application of acid hydrolysis technology.Germany developed the diluted acid lixiviation process in 1932, i.e. Scholler process, and this device is very simple, just dilute acid soln is pumped into the wood chip bed; In World War II, U.S.'s Forest Products Laboratory (FPL) has improved Schollerprocess, produce Madison wood sugar process technology, throughput increases substantially, after through the repeatedly improvement of TVA etc., nineteen fifty-two has been put into effect dilute acid hydrolysis diafiltration bed bioreactor (percolationreactor), is still biomass saccharification one of the simplest method at present, and becomes the benchmark of invention novel method.
The early stage later stage seventies to the eighties in 20th century, about the model and the experimental study of dilute acid hydrolysis system becomes focus, by kinetic model research and technological design practice, the investigator recognizes high solids concn, and the countercurrent flow of solid-liquid and the short residence time are the keys that improves sugared yield; Nineteen eighty-three proposes the two-stage dilute acid hydrolysis process by Stinson, and its principle is different with cellulosic hydrolysising condition according to hemicellulose, separates hydrolysis with different reaction conditionss; Study focus over past ten years and be to develop new reactor and theoretical model thereof to improve the dilute acid hydrolysis productive rate; Seek new hydrolysis process, as the hydrolysis of ultralow density acid, organic acid hydrolysis etc.; To influence factor and the more deep research of hydrolysis mechanism.Novel reactor mainly contains the adverse current hydrolysis, shrinks the bed hydrolysis, cross-stream hydrolysis and combination thereof etc.
The patent of domestic relevant cellulose series biomass hydrolysis reactor research mainly contains: the CN1624076A apparatus for preparing liquid fuel by biological matter ultra-low acid hydrolyzing, ZL200720054772.9 cellulose series biomass hydrolysis device, the method for CN1927874A preparing monosaccharide with diluent acid continuous catalyzing biomass and device thereof.Preceding two patents are extremely low acids hydrolysis batch reactor and compression percolating device, can only realize reaction and semicontinuous reaction intermittently, and efficient is low, are difficult to engineering and use; The 3rd patent realized the continuous diluted acid catalytic hydrolysis of biomass single stage method, because of the acid hydrolysis of biomass, is consecutive reaction, and carbohydrate is an intermediate product, adopts the single stage method hydrolysis, is difficult to the further degraded of control carbohydrate product, influences the effect of hydrolysis.
Summary of the invention
The object of the present invention is to provide a kind of method and the device thereof that can realize two step continuous hydrolysis of cellulose series biomass, react sugared yield to improve, and help the utilization of collection respectively of product, for its industrializing implementation is made place mat.
For realizing above purpose, the present invention has taked following technical scheme: the method for cellulose series biomass continuous hydrolysis comprises the steps:
(1) the solid biomass mass transport that will be mixed with moisture is in the interior horizontal piston flow reactor that is provided with the variable-pitch auger catch bar;
(2) simultaneously the reaction solution of ultralow acid or high temperature liquid water is input in the horizontal piston flow reactor, the mixture of solid biomass material and reaction solution advances under the promotion of variable-pitch auger catch bar;
(3) said mixture at 180-220 ℃, reacts under the condition of 3.0-4.0MPa in horizontal piston flow reactor, realizes solid-liquid separation by the varying pitch squeezing then;
(4) solid residue is input to the vertical countercurrent reactor, upwards carries by the uniform pitch vertical helical catch bar in the vertical countercurrent reactor, imports ultralow acid-respons liquid simultaneously from the top of vertical countercurrent reactor, realizes countercurrent reaction;
(5) collect solid residue on the top of vertical countercurrent reactor at last, cellulosic hydrolysate is collected in the bottom.This solid biomass material is the mixture of hemicellulose, Mierocrystalline cellulose and xylogen.
Include continuously feeding air lock system, horizontal piston flow reactor, vertical countercurrent reactor, be provided with the variable-pitch auger catch bar in the described horizontal piston flow reactor, it comprises feed zone, main reaction section and squeeze section, this feed zone is communicated with described continuously feeding air lock system, be connected with the residue e Foerderanlage on an end of the horizontal piston flow reactor behind the squeeze section, this residue e Foerderanlage the other end is communicated with described vertical countercurrent reactor.
Be provided with uniform pitch vertical helical catch bar in the described vertical countercurrent reactor, be provided with the reaction solution shower nozzle in this reactor head.
Be communicated with by the raw material pre-mixing apparatus between described continuously feeding air lock system and the horizontal piston flow reactor, also include the product liquid collector that is connected with described squeeze section.The product liquid collector is used for reacted product liquid is collected, and makes solid residue can enter into follow up device more convenient, more fully.
Between described squeeze section and product liquid collector, be connected with refrigerating unit.The setting of refrigerating unit can be used for rapid cooling, termination reaction.
The residue drawing mechanism that described vertical countercurrent reactor upper end is provided with the reaction residues collector and is communicated with it.The residue drawing mechanism is used for the reaction residues thing in final reaction stage is collected.
Be provided with thermal insulation layer at described horizontal piston flow reactor and vertical countercurrent reactor skin.Thermal insulation layer the constant temperature of reaction that can guarantee reactor is set.
The screw-blade of described residue e Foerderanlage, residue drawing mechanism adopts saw-toothed blade.Saw-toothed blade has good stirring and loose effect, is beneficial to material reaction uniformity in reactor.
Cellulose series biomass continuous hydrolysis method by the hemicellulose in the biomass and Mierocrystalline cellulose under different condition respectively continuous hydrolysis improve the sugared yield of reaction.
The present invention compared with prior art has following advantage:
1, adopt two one-step hydrolysis methods, the difference continuous hydrolysis under different condition hemicellulose in the biomass and Mierocrystalline cellulose has been avoided the further degraded of hydrolysate, has improved hydrolysis effect.
2, adopt the piston flow reactor hydrolyzed hemicellulose, its hydrolytic process and result all are better than traditional pot type stirred reactor.Mierocrystalline cellulose hydrolysis in the vertical countercurrent reactor, treatment effect is better than co-current reactor.
3, whole cellulose series biomass continuous hydrolysis device has comprised feeding system, biomass by hydrolyzation reactive system and product collection system, has realized real operate continuously.
Description of drawings
Fig. 1 is a cellulose series biomass continuous hydrolysis device synoptic diagram;
Fig. 2 variable-pitch auger catch bar synoptic diagram;
Description of reference numerals: 1, continuously feeding air lock system, 2, horizontal piston flow reactor, 3, the vertical countercurrent reactor, 4, product liquid collector, 5, the reaction residues collector, 6, the residue e Foerderanlage, 7, reaction solution shower nozzle, 8, raw material pre-mixing apparatus, 9, thermal insulation layer, 10, refrigerating unit, 11, uniform pitch vertical helical catch bar, 12, residue drawing mechanism, 13, the variable-pitch auger catch bar, 14, the cellulose hydrolysis collection.
Embodiment
Below in conjunction with the drawings and specific embodiments content of the present invention is described in further details.
Embodiment:
As shown in Figure 1, the present embodiment device comprises that the continuous hydrolysis device is made up of feeding system, biomass by hydrolyzation reactive system and product collection system, and wherein feeding system is realized to the High Temperature High Pressure charging by a spherical gas locking device; Reactive system comprises the piston flow reactor of hydrolysis of hemicellulose and the vertical countercurrent reactor of cellulose hydrolysis; Product collection system comprises the collection of product liquid and solid residue.
Specifically include continuously feeding air lock system 1, horizontal piston flow reactor 2, vertical countercurrent reactor 3.In the horizontal piston flow reactor 2 is variable-pitch auger catch bar 13, comprises feed zone A, main reaction section B and squeeze section C.Be provided with the reaction-ure feeding mouth at feed zone A, be communicated with continuously feeding air lock system 1, squeeze section C is provided with the product discharge port, and is connected with residue e Foerderanlage 6.
Be communicated with by raw material pre-mixing apparatus 8 between continuously feeding air lock system 1 and the horizontal piston flow reactor 2, also include the product liquid collector 4 that is connected with described squeeze section C, and between squeeze section C and product liquid collector 4, be connected with refrigerating unit 10
In the vertical countercurrent reactor 3 is uniform pitch vertical helical catch bar 11, is provided with reaction solution shower nozzle 7 in reactor head.The top is provided with residue drawing mechanism 12 and reaction residues collector 5 simultaneously, is provided with cellulose hydrolysis collection 14 (include refrigerating unit 10, can charge into high pressure nitrogen in this refrigerating unit to guarantee cryogenic effect) in the bottom.Wherein residue e Foerderanlage 6 and residue drawing mechanism 12 adopt segment helical feed mode, and revolution speed of screw adopts the frequency modulation variator to regulate, and screw-blade adopts saw-toothed blade; And can connect water coolant on the reaction residues collector 5 to guarantee the low temperature in the collector.
With the straw is that hydrolysis material is an example, the straw the pulverized continuously feeding air lock system 1 by ball-type is sent to raw material pre-mixing apparatus 8, mix with the reaction solution of the high temperature liquid water that flows into, be pressed into horizontal piston flow reactor 2 reactions then, squeeze through squeeze section C, reacted hemicellulose hydrolysate enters product liquid collector 4, simultaneously through its refrigerating unit 10 coolings, and reaction residues is pushed into residue e Foerderanlage 6, be sent to vertical countercurrent reactor 3 at last, promoted to rise by uniform pitch vertical helical catch bar 11 spirals, thereby the liquid that responds simultaneously in the process that residue is upwards carried is realized the countercurrent reaction of vertical countercurrent reactor 3 from top reaction solution shower nozzle 7 ejections of vertical countercurrent reactor 3.Reaction finishes the back residue and releases reaction residues collector 5 by the residue drawing mechanism 12 at reactor 3 tops, spray simultaneously is the cold water cooling down, and hydrolysis reaction liquid is collected through the cellulose hydrolysis collection 14 of vertical countercurrent reactor 3 bottoms, simultaneously through its refrigerating unit cooling.
What adopt among the present invention is lignocellulose-like biomass, comprises the fiber substances such as paper of agriculture and forestry organic waste material, careless class and recovery such as timber, wood chip, agricultural crop straw.Be provided with flange at the head end of this variable-pitch auger catch bar and fix, and rotate by thrust block and this catch bar of driven by motor.
Above-listed detailed description is at the specifying of possible embodiments of the present invention, and this embodiment is not in order to limiting claim of the present invention, and the equivalence that all the present invention of disengaging do is implemented or change, all should be contained in the claim of this case.
Claims (5)
1. the method for cellulose series biomass continuous hydrolysis is characterized in that, comprises the steps:
(1) the solid biomass mass transport that will be mixed with moisture is in the interior horizontal piston flow reactor that is provided with the variable-pitch auger catch bar;
(2) simultaneously the reaction solution of ultralow acid or high temperature liquid water is input in the horizontal piston flow reactor, the mixture of solid biomass material and reaction solution advances under the promotion of variable-pitch auger catch bar;
(3) said mixture at 180-220 ℃, reacts under the condition of 3.0-4.0MPa in horizontal piston flow reactor, realizes solid-liquid separation by the varying pitch squeezing then;
(4) solid residue is input to the vertical countercurrent reactor, upwards carries by the uniform pitch vertical helical catch bar in the vertical countercurrent reactor, imports ultralow acid-respons liquid simultaneously from the top of vertical countercurrent reactor, realizes countercurrent reaction;
(5) collect solid residue on the top of vertical countercurrent reactor at last, cellulosic hydrolysate is collected in the bottom.
2. the method for cellulose series biomass continuous hydrolysis as claimed in claim 1 is characterized in that: described solid biomass material is the mixture of hemicellulose, Mierocrystalline cellulose and xylogen.
3. cellulose series biomass continuous hydrolysis device, it is characterized in that: include continuously feeding air lock system (1), horizontal piston flow reactor (2), vertical countercurrent reactor (3), be provided with variable-pitch auger catch bar (13) in the described horizontal piston flow reactor (2), it comprises feed zone (A), main reaction section (B) and squeeze section (C), this feed zone (A) is communicated with described continuously feeding air lock system (1), be communicated with by raw material pre-mixing apparatus (8) between described continuously feeding air lock system (1) and the horizontal piston flow reactor (2), also include the product liquid collector (4) that is connected with described squeeze section (C), between described squeeze section (C) and product liquid collector (4), be connected with refrigerating unit (10); Be connected with residue e Foerderanlage (6) on an end of the horizontal piston flow reactor (2) behind the squeeze section (C), this residue e Foerderanlage (6) the other end is communicated with described vertical countercurrent reactor (3); Be provided with uniform pitch vertical helical catch bar (11) in the described vertical countercurrent reactor (3), be provided with reaction solution shower nozzle (7) at this reactor (3) top; The residue drawing mechanism (12) that described vertical countercurrent reactor (3) upper end is provided with reaction residues collector (5) and is communicated with it.
4. cellulose series biomass continuous hydrolysis device as claimed in claim 3 is characterized in that: be provided with thermal insulation layer (9) at described horizontal piston flow reactor (2) and vertical countercurrent reactor (3) skin.
5. cellulose series biomass continuous hydrolysis device as claimed in claim 4, it is characterized in that: described residue e Foerderanlage (6), residue drawing mechanism (12) adopt segment helical feed mode, revolution speed of screw adopts the frequency modulation variator to regulate, and screw-blade adopts saw-toothed blade.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768538B (en) * | 2010-01-14 | 2013-01-23 | 中国科学院广州能源研究所 | Horizontal multi-helix biomass continuous hydrolysis and saccharification device and method |
| CN101818217B (en) * | 2010-05-06 | 2012-12-26 | 中国科学院广州能源研究所 | Method and device for pretreatment of high-temperature liquid water of cellulosic biomass |
| CN102021252B (en) * | 2010-12-21 | 2013-02-27 | 山东省鲁洲食品集团有限公司 | Method and device for continuously hydrolyzing corn bran |
| CN102677503B (en) * | 2012-05-29 | 2016-04-27 | 中国科学院过程工程研究所 | A kind of living beings continuous hydrothermal pre-treatment reactor |
| CN102690898B (en) * | 2012-06-15 | 2013-09-25 | 王建设 | Continuous hydrolysis device and method for cellulose straw materials |
| RU2592777C1 (en) * | 2015-03-24 | 2016-07-27 | Общество с ограниченной ответственностью "Научно-технический центр Гринтекс" (ООО "НТЦ Гринтекс") | Installation for continuous production of powdered cellulose |
| CN107447057B (en) * | 2016-05-31 | 2021-08-03 | 中国科学院大连化学物理研究所 | Biomass continuous hydrolysis and compression molding device |
| CN107447059A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院大连化学物理研究所 | A kind of biomass by hydrolyzation produces xylose mother liquid and residue compression forming integral method |
| CN107356706B (en) * | 2017-05-31 | 2019-10-22 | 中国科学技术大学 | A kind of method of continuity method measurement biomass by hydrolyzation kinetics |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624076A (en) * | 2004-10-25 | 2005-06-08 | 浙江大学 | Apparatus for preparing liquid fuel by biological matter ultra-low acid hydrolyzing |
| CN1927874A (en) * | 2006-09-27 | 2007-03-14 | 华东理工大学 | Method and apparatus for preparing monosaccharide with diluent acid continuous catalyzing biomass |
| CN101120102A (en) * | 2005-02-15 | 2008-02-06 | 奥克西特诺工业与贸易公司 | Acid hydrolysis process of cellulosic and lignocellulosic materials, digestion vessel and hydrolysis reactor |
| CN201077823Y (en) * | 2007-07-27 | 2008-06-25 | 中国科学院广州能源研究所 | Cellulose biomass hydrolyzing device |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624076A (en) * | 2004-10-25 | 2005-06-08 | 浙江大学 | Apparatus for preparing liquid fuel by biological matter ultra-low acid hydrolyzing |
| CN101120102A (en) * | 2005-02-15 | 2008-02-06 | 奥克西特诺工业与贸易公司 | Acid hydrolysis process of cellulosic and lignocellulosic materials, digestion vessel and hydrolysis reactor |
| CN1927874A (en) * | 2006-09-27 | 2007-03-14 | 华东理工大学 | Method and apparatus for preparing monosaccharide with diluent acid continuous catalyzing biomass |
| CN201077823Y (en) * | 2007-07-27 | 2008-06-25 | 中国科学院广州能源研究所 | Cellulose biomass hydrolyzing device |
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