CN104073533A - Method for preprocessing biomass through thermal hydrolysis with low energy consumption and device thereof - Google Patents
Method for preprocessing biomass through thermal hydrolysis with low energy consumption and device thereof Download PDFInfo
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Abstract
The invention provides a method for preprocessing biomass through thermal hydrolysis with low energy consumption and a device applied to the method. By virtue of the method, a thermal hydrolysis processing manner with high concentration of substrate and low hydrolysis temperature is used, integrated with an ultrasonic processing manner and used for preprocessing a lignocelluloses biomass raw material and reusing a hydrolysis liquid of hydrolysis reaction; the water consumption in the preprocessing process through thermal hydrolysis is reduced in the condition without influence on the hydrolysis efficiency of solid residue enzyme; moreover, the yield and concentration of monosaccharide in the hydrolysis liquid are improved; and meanwhile, the hydrolysis residue with high content of solid is obtained, so that the increase of the concentration of saccharide of enzyme hydrolysis in the later period can be facilitated. The method has the advantages of low water consumption, low heat consumption, energy conservation, environmental protection and high yield of target products, and the like. The invention provides a device applied to the method for preprocessing biomass. The device has the advantages of simple structure and easiness in operation, and the like.
Description
Technical field
The present invention relates to the technical field that Wood Adhesives from Biomass becomes new forms of energy, particularly a kind of method of thermal hydrolysis means preprocessing lignocellulose biolobic material and device of applicable the method for utilizing.
Background technology
Lignocellulose-like biomass diastatic fermentation is produced the high valuable chemicals such as the biological alcohol liquid fuels such as alcohol fuel, butanols, amylalcohol and Xylitol, lactic acid, succsinic acid, for development energy substitution, safeguard national energy security, alleviate environmental pollution etc. and have very important meaning.Yet in lignocellulosic material, the component such as natural cellulose and hemicellulose, xylogen has formed extremely complicated three-dimensional structure, and this dense structure by formation such as chemical bond, hydrogen bond, hydrophobic interactions has seriously hindered microbial transformation.By preconditioning technique, break Mierocrystalline cellulose-hemicellulose-lignin structure closely, reduce cellulosic degree of crystallinity and the polymerization degree, remove the steric hindrance of xylogen, increase material surface apertures and surface-area, most important for the polysaccharide utilization ratio that improves biomass cellulose enzyme enzymatic hydrolyzation and follow-up microorganism.
High temperature liquid water (Liquid Hot Water) refers to that temperature is between 150 ℃-350 ℃, and pressure is higher than the compressed liquid water of its saturated vapor pressure.High temperature liquid water is except (temperature is greater than 374 ℃ with supercritical water, pressure is higher than 22Mpa) equally have outside the feature of mass-transfer performance good (low-viscosity and high spread coefficient), self also has the function of acid catalysis and base catalysis, in addition, relatively postcritical condition, its reaction conditions milder, more easily controls and realizes industrialization.
Compare with pretreatment processs such as traditional acid-base method, the explosions of ammonia fiber, high temperature liquid water preprocessing process is used green cheap reaction medium, do not need to add any chemical reagent, there is higher hemicellulose derived carbohydrate yield, cellulase hydrolysis rate and lower degraded product production rate, because becoming the study hotspot of preprocessing technical field.By retrieving domestic relevant patent documentation, Patents about hot liquid water processing lignocellulosic material comprises at present: CN101268121A (proprietary term: the method and apparatus that cellulose materials is changed into ethanol), disclose at 170-230 ℃ filamentary material has been carried out to hydrothermal pretreatment, and laid particular emphasis on a kind of method for fuel ethanol production and relevant device are provided.CN101736631A (proprietary term: a kind of technique of efficiently preprocessing lignocellulose), disclose the employing method of fractional steps lignocellulose has been carried out to pre-treatment, first in the overcritical superheated water of 160-250 ℃, boiling obtains hemicellulose oligosaccharides, afterwards it is carried out to flash distillation under diluted acid environment and obtains fermentability monose.CN101818217A (proprietary term: a kind of pretreated method of high-temperature liquid water of cellulosic biomass and device), the method and the device thereof that provide high temperature liquid water (150-200 ℃) that a kind of employing contains metal ion to be hydrolyzed to lignocellulose-like biomass.CN101586136A (proprietary term: a kind of method of high-efficiency pretreatment on biomass), provide a kind of employing two step alternating temperature segmentations (first 160-200 ℃ processing, then 200-260 ℃ of processing) high temperature liquid water to carry out pretreated method to lignocellulose-like biomass.CN102517403A (proprietary term: a kind of method of utilizing high temperature liquid water to prepare hemicellulose oligose), provide a kind of method of utilizing high temperature liquid water to prepare hemicellulose oligose.Visible, high-temperature liquid state water pretreatment at present is mostly carried out the in the situation that of High Temperature High Pressure, low concentration of substrate, it is unfavorable that research shows low temperature, low water usage amount is processed for the enzymic hydrolysis rate that improves biomass residue, and high energy consumption drops into and limited its applying in lignocellulose-like biomass diastatic fermentation field.
Summary of the invention
The invention provides a kind of thermal hydrolysis biomass pretreatment method and device thereof of low power consuming, the method is not in the situation that affecting solid residue enzymic hydrolysis efficiency, reduce the water consumption in hydrolysis preprocessing process, and improved monose yield and concentration in hydrolyzed solution, the hydrolytic residue that simultaneously obtains high solids content is convenient to the raising of late enzyme hydrolysis sugar concentration.
A thermal hydrolysis biomass pretreatment method for low power consuming, comprises the following steps:
Step 1, thermal hydrolysis are processed: granularity is less than to 1cm lignocellulose-like biomass raw material as in hydrolysis reactor, is not less than 20% adds after water according to quality of material concentration, stir, 100-180 ℃ of Water Under solution, the reaction times is 5-60min;
Step 2, supersound process: the solidliquid mixture of step 1 gained is added water to quality of material concentration lower than 5%, is that 20-60kHz, power are supersound process 5-60min under the condition of 50-500w, temperature 20-100 ℃ in ultrasonic frequency;
Step 3, will step 2 gained solid product dehydration after carry out high solids content enzymic hydrolysis; By every gram of substrate, add 10-30FPU lytic enzyme, at pH4.8 Water Under solution 72h; In wherein said high solids content enzymic hydrolysis, substrate mass concentration is not less than 20%;
Step 4, the hydrolyzed solution of collecting step 2 gained circulation are as the reaction solution of new round hydrolysis reaction.
Preferably, in the thermal hydrolysis treating processes of described step 1, according to the character of different biomass materials, in reactor, pass into a kind of in ammonia, carbonic acid gas, sulfurous gas, oxygen, air, nitrogen, making reaction environment is alkalescence or acidity or oxidation or inert environments.
Preferably, the hydrolyzed solution that described step 4 is collected is to be recovered in the reactor of step 1 by volume pump.
Particularly, described lignocellulose-like biomass raw material is agriculture forestry waste, comprise sweet sorghum slag, bagasse, corn cob, maize straw, Wheat Straw, straw, energy grass, etc.
The present invention also provides a kind of device that is applicable to the thermal hydrolysis biomass pretreatment method of above-mentioned low power consuming, and this device comprises hydrolytic decomposition pot, aftertreatment tank, water knockout and splice jug; The discharge port of described hydrolytic decomposition pot is connected with the opening for feed of aftertreatment tank, and aftertreatment tank is connected with water knockout and splice jug respectively; On described splice jug, be also provided with the pipeline being communicated with hydrolytic decomposition pot; Described aftertreatment tank is provided with ultrasonic transducer.
Preferably, described hydrolytic decomposition pot adopts circulating-heating oil rapid heating.The structure of hydrolytic decomposition pot is jacketed type heating tank, main tank body and the external placed type heating jacket assembly that is arranged on main tank body periphery, consists of; Described external placed type heating jacket assembly comprises chuck layer and heating/cooling oil box, and chuck layer and heating/cooling oil box are connected to form the path of circulation by pipeline; Between described heating/cooling oil box and pipeline, be also provided with T-valve.After reaction finishes, by the switching of T-valve, can make cooling oil cooling fast.
Preferably, on the pipeline of described connection splice jug and hydrolytic decomposition pot, be also provided with volume pump.
Preferably, described water knockout is press type water knockout or centrifugal dewatering tank.
The key innovation of apparatus of the present invention is: (1) design hydrolyzed solution cyclically utilizing link, reduced whole process water consumption, and improved monose yield simultaneously.(2) design supersound process link, has realized the combination of high concentration of substrate pre-treatment and high residue enzymatic hydrolyzation.(3) design solid residue dehydration link, the hydrolytic residue that obtains high solids content is convenient to improve late enzyme hydrolysis sugar concentration.(4) whole low power consuming pretreatment unit has been realized high material concentration, low reaction temperatures hydrolysis, ultrasonic aftertreatment, dehydration and hydrolyzed solution reusing integral, adopts thermal oil to replace electrically heated, realizes rapid heating and cooling.
Technical scheme of the present invention has following advantage: (1), by hydrolyzed solution cyclically utilizing, has reduced whole process water consumption, has improved monose yield simultaneously.(2) material concentration is higher than general high temperature liquid water hydrolysis temperature is low for the temperature that pyrohydrolysis process adopts, more energy-conservation than traditional hydrolysis process for treating.(3) by supersound process, realized the combination of high concentration of substrate pre-treatment and high residue enzymatic hydrolyzation.(4) solid residue is through processed, and the hydrolytic residue that obtains high solids content is convenient to improve late enzyme hydrolysis sugar concentration.(5) whole low power consuming pretreatment unit has been realized hydrolysis, ultrasonic aftertreatment, dehydration and hydrolyzed solution reusing integral, adopts thermal oil to replace electrically heated, realizes rapid heating and cooling.
The inventive method has adopted the thermal hydrolysis processing means of high concentration of substrate and low in hydrolysis temperature and combined supersound process means carries out pre-treatment to lignocellulose-like biomass raw material, and by the hydrolyzed solution of hydrolysis reaction again reuse.The method has the advantages such as low water consumption, low heat dissipation, energy-saving and environmental protection, target product high yield.The device that is applicable to above-mentioned biomass pretreatment method provided by the invention on the other hand, have simple in structure, the advantage such as be easy to control.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention 1 device.
Reference numeral: 1-hydrolytic decomposition pot; 2-aftertreatment tank; 3-water knockout; 4-splice jug; Under 6-, open up valve; 7-volume pump; 8-ultrasonic transducer;
The main tank body of 11-; 12-chuck layer; 13-heating/cooling oil box; 14-circulating oil pump; 15-T-valve; 16-safety valve.
Embodiment
Below provide the structure implemented of apparatus of the present invention, and in conjunction with device of the present invention, provide the thermal hydrolysis biomass pretreatment method embodiment of low power consuming:
Embodiment 1:
A thermal hydrolysis biomass pretreatment unit for low power consuming, its structure as shown in Figure 1: mainly comprise hydrolytic decomposition pot 1, aftertreatment tank 2, water knockout 3, splice jug 4; Described aftertreatment tank 2 is placed in the below of hydrolytic decomposition pot 1, and the discharge port of hydrolytic decomposition pot 1 is connected by lower exhibition valve 6 with the opening for feed of aftertreatment tank 2; Described water knockout 3 is placed in the below of aftertreatment tank 2, and the discharge port of aftertreatment tank 2 is also connected by lower exhibition valve with the opening for feed of water knockout 3, and solid residue enters water knockout 3 and dewaters after aftertreatment; Near the discharge port of described aftertreatment tank 2, be also provided with the pipeline being connected with splice jug 4 tops; The bottom of splice jug 4 is also communicated with hydrolytic decomposition pot 1 by pipeline, and is also provided with volume pump 7 on the pipeline being communicated with, and realizes hydrolyzed solution cyclically utilizing.Described aftertreatment tank 2 is provided with ultrasonic transducer 8.
Described hydrolytic decomposition pot 1 is jacketed type heating tank, main tank body 11 and external placed type heating jacket assembly, consists of; Described external placed type heating jacket assembly comprises chuck layer 12, heating/cooling oil box 13 and circulating oil pump 14, and chuck layer 12, heating/cooling oil box 13 and circulating oil pump 14 are connected to form the path of circulation by pipeline; Near described heating/cooling oil box 13, be also provided with T-valve 15, T-valve 15 is for regulating deep fat or cooling oil enters.On described hydrolytic decomposition pot 1, be also provided with safety valve 16.
Embodiment 2:
Take corn cob as raw material, be crushed to granularity and be less than 1cm, directly drop in the hydrolysis reactor in pretreatment unit, after adding water according to quality of material concentration 25%, stir, 100 ℃ of Water Under solutions, the reaction times is 60min, and in process, passing into nitrogen, to maintain system pressure be 2MPa.After thermal hydrolysis processing finishes, the solid-liquid mixture in hydrolysis reactor is discharged in aftertreatment tank, adding water, to make its solid masses concentration be 5%, in ultrasonic frequency, is 20kHz, and power is 50w, processes 60min at 20 ℃.After processing, collect liquid product in splice jug, main containing 90% xylo-oligosaccharide, 5% monose (comprising wood sugar and pectinose) in this product, other compositions are sugared degraded product (furfural, formic acid, acetic acid etc.).The further unloading of solid materials is in water knockout, after dehydration, solid materials water ratio is 75%, add cellulolytic enzyme directly to carry out high solids content enzymic hydrolysis, condition is substrate mass concentration 20%, enzyme concentration 10FPU/g, pH4.8,50 ℃, under 150rpm condition, after enzymolysis 72h, cellulase hydrolysis rate is 85%, is about 2 times (thermal hydrolysis treatment condition are identical) of not carrying out aftertreatment residue enzymatic hydrolyzation.Hydrolyzed solution in splice jug is back to use in hydrolytic decomposition pot by volume pump, with next batch solid materials mixed hydrolysis, and 1 times of whole process water saving, hydrolyzed solution xylose concentration improves 2 times simultaneously, is 20g/l.This embodiment be equally applicable to rice husk, palm hull, etc. agricultural and sideline waste.
Embodiment 3:
The discarded bagasse in sugar refinery of take is raw material, be crushed to granularity and be less than 1cm, directly drop in the hydrolysis reactor in pretreatment unit, after adding water according to quality of material concentration 20%, stir, 160 ℃ of Water Under solutions, reaction times is 30min, and in process, passing into ammonia, to maintain system pressure be 2MPa.After thermal hydrolysis processing finishes, the solid-liquid mixture in hydrolysis reactor is directly discharged in aftertreatment tank, and adding water, to make its solid masses concentration be 4%, in ultrasonic frequency, is 30kHz, and power is 300w, under temperature 50 C, processes 30min.After processing, collect liquid product in splice jug, main containing 70% xylo-oligosaccharide, 8% monose (comprising wood sugar, glucose and pectinose) in this product, other composition is sugared degraded product (as furfural) and lignin degradation product (as coumaric aldehyde, p-Hydroxybenzaldehyde etc.).The further unloading of solid materials is in water knockout, after dehydration, be about 75% to body material water ratio, add cellulolytic enzyme, by residue in substrate mass concentration 20%, enzyme concentration 30FPU/g, pH4.8,50 ℃, under 150rpm condition, after enzymolysis 72h, cellulase hydrolysis rate is 62%, is about 2.6 times (thermal hydrolysis treatment condition are identical) of not carrying out aftertreatment residue enzymatic hydrolyzation.Hydrolyzed solution in splice jug is back to use in hydrolytic decomposition pot by volume pump, with next batch solid materials mixed hydrolysis, and 1 times of whole process water saving, hydrolyzed solution xylose concentration improves 1.2 times simultaneously, is 8g/l.The method be equally applicable to sweet sorghum slag, maize straw, Wheat Straw, straw, etc. stalk biomass raw material.
Embodiment 4:
Take wolf grass as raw material, be crushed to granularity and be less than 1cm, directly drop in the hydrolysis reactor in pretreatment unit, stir after adding water according to mass concentration 20%, 180 ℃ of Water Under solutions, the reaction times is 5min, keeps saturated vapor pressure in process.After thermal hydrolysis finishes, solid-liquid mixture in hydrolysis reactor is discharged in aftertreatment tank, adding water, to make its solid masses concentration be 5%, in ultrasonic frequency, be 60kHz, power is 500w, at 100 ℃, process 5min, after processing, collect liquid product in splice jug, main containing 80% xylo-oligosaccharide in this product, 10% monose (comprises wood sugar, glucose and pectinose), other compositions are sugared degraded product (furfural, 5 hydroxymethyl furfural, formic acid, acetic acid etc.) and lignin degradation product (as coumaric acid, forulic acid, P-hydroxybenzoic acid, coumaric aldehyde, p-Hydroxybenzaldehyde etc.).The further unloading of solid materials is in water knockout, after dehydration, solid materials water ratio is 75%, add cellulolytic enzyme, condition is substrate mass concentration 20%, enzyme concentration 20FPU/g, pH4.8,50 ℃, under 150rpm condition, after enzymolysis 72h, cellulase hydrolysis rate is 75%, is about 2.3 times (thermal hydrolysis treatment condition are identical) of not carrying out aftertreatment residue enzymatic hydrolyzation.Hydrolyzed solution in splice jug is back to use in hydrolytic decomposition pot by volume pump, with next batch solid materials mixed hydrolysis, and 1 times of whole process water saving, hydrolyzed solution xylose concentration improves 1.5 times simultaneously, is 10g/l.The method is equally applicable to switchgrass, napier grass, equal energy source grass as raw material.
Claims (8)
1. a thermal hydrolysis biomass pretreatment method for low power consuming, is characterized in that, comprises the following steps:
Step 1, thermal hydrolysis are processed: the lignocellulose-like biomass raw material that granularity is less than to 1cm, as in hydrolysis reactor, is not less than 20% according to quality of material concentration and adds after water, stirs, and 100-180 ℃ of Water Under solution, the reaction times is 5-60min;
Step 2, supersound process: the solidliquid mixture of step 1 gained is added water to quality of material concentration lower than 5%, is that 20-60kHz, power are supersound process 5-60min under the condition of 50-500w, temperature 20-100 ℃ in ultrasonic frequency;
Step 3, will step 2 gained solid product dehydration after carry out high solids content enzymic hydrolysis; By every gram of substrate, add 10-30FPU lytic enzyme, at pH4.8 Water Under solution 72h; In wherein said high solids content enzymic hydrolysis, substrate mass concentration is not less than 20%;
Step 4, the hydrolyzed solution of collecting step 2 gained circulation are as the reaction solution of new round hydrolysis reaction.
2. the thermal hydrolysis biomass pretreatment method of low power consuming as claimed in claim 1, it is characterized in that, in the thermal hydrolysis treating processes of described step 1, also can in reactor, pass into a kind of in ammonia, carbonic acid gas, sulfurous gas, oxygen, air, nitrogen, making reaction environment is alkalescence or acidity or oxidation or inert environments.
3. the thermal hydrolysis biomass pretreatment method of low power consuming as claimed in claim 1, is characterized in that, the hydrolyzed solution that described step 4 is collected is to be recovered in the reactor of step 1 by volume pump.
4. the thermal hydrolysis biomass pretreatment method of low power consuming as claimed in claim 1, it is characterized in that, described lignocellulose-like biomass raw material is agriculture forestry waste, is selected from sweet sorghum slag, bagasse, corn cob, maize straw, Wheat Straw, straw, energy grass.
5. a device that is applicable to the thermal hydrolysis biomass pretreatment method of the low power consuming described in claim 1-4 any one, is characterized in that: this device comprises hydrolytic decomposition pot, aftertreatment tank, water knockout and splice jug; The discharge port of described hydrolytic decomposition pot is connected with the opening for feed of aftertreatment tank, and aftertreatment tank is connected with water knockout and splice jug respectively; On described splice jug, be also provided with the pipeline being communicated with hydrolytic decomposition pot; Described aftertreatment tank is provided with ultrasonic transducer.
6. device as claimed in claim 5, is characterized in that, described hydrolytic decomposition pot is jacketed type heating tank, main tank body and the external placed type heating jacket assembly that is arranged on main tank body periphery, consists of; Described external placed type heating jacket assembly comprises chuck layer, heating/cooling oil box and circulating oil pump, and chuck layer, heating/cooling oil box and circulating oil pump are connected to form the path of circulation by pipeline; Near described heating/cooling oil box, be also provided with T-valve.
7. device as claimed in claim 5, is characterized in that, on the pipeline of described connection splice jug and hydrolytic decomposition pot, is also provided with volume pump.
8. device as claimed in claim 5, is characterized in that, described water knockout is press type water knockout or centrifugal dewatering tank.
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| CN105063132A (en) * | 2015-08-27 | 2015-11-18 | 福建农林大学 | Method for improving fermentable sugar generating efficiency through bamboo cellulose high-concentration enzymatic hydrolysis |
| CN105112459A (en) * | 2015-09-23 | 2015-12-02 | 大连工业大学 | Lignocellulose biomass circulating, strengthening and pre-hydrolyzing process |
| CN105410948A (en) * | 2015-12-10 | 2016-03-23 | 广东省农业科学院蚕业与农产品加工研究所 | Water-soluble radix puerariae fiber oligosaccharide and preparing method thereof |
| CN106191327A (en) * | 2016-08-31 | 2016-12-07 | 中国科学院广州能源研究所 | A kind of response system utilizing carbon-based solid acid catalyst two-step hydrolysis biomass |
| 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 |
| WO2018023474A1 (en) * | 2016-08-03 | 2018-02-08 | 江苏思佳生物质科技有限公司 | Method, catalyst and equipment for degrading biomass |
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| 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 |
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