CN102816811B - Method for pre-treating biomass by means of microwave dry method or semidry method - Google Patents
Method for pre-treating biomass by means of microwave dry method or semidry method Download PDFInfo
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- CN102816811B CN102816811B CN201110154426.9A CN201110154426A CN102816811B CN 102816811 B CN102816811 B CN 102816811B CN 201110154426 A CN201110154426 A CN 201110154426A CN 102816811 B CN102816811 B CN 102816811B
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- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a method for pre-treating biomass by means of a microwave dry method or a semidry method. The method is characterized by comprising the steps of smashing materials to be particles with particle size of 1-50mm, adjusting moisture content of the materials to reach 10-30%(w/w), placing the materials in a microwave heating device, adopting power of 50-1000w/kg of wet feed to preheat, adjusting heating power to be the power of 1-5kw/kg of wet feed after the material temperature rises to 95-98 DEG C, performing quick heating till the temperature rises to 130-150 DEG C, retaining the temperature for 10-1000 seconds and then stopping heating, and finishing one pre-treatment, wherein treated raw materials can be treated for one to three times to enhance the treatment effect according to different requirements after the moisture content is adjusted. The method adopts microwave to pre-treat the biomass, controls the temperature by controlling the moisture content of the materials, enables the treating temperature to reach to 130-150 DEG C on the premise that a pressure container is not utilized, enhances the treatment effect, is short in treatment time, low in investment, obvious in treatment effect and does not produce fermentation inhibitors.
Description
Technical field
The invention belongs to biomass preprocessing technical field, particularly the method for the dry or semidrying preprocessing biomass of a kind of microwave.
Background technology
Along with the exhaustion day by day of petrochemical industry resource, substitute petrochemical industry resource with reproducible biomass resource, be biomass energy by biorefinery technology by Wood Adhesives from Biomass, biomass chemical and biological material are developing direction from now on, are also to solve the inevitable means of human environment, resource and energy problem from now on.Biorefinery, taking the production of bioenergy as example, its basic procedure is: biomass collection, biomass pre-treatment, cellulase hydrolysis, ethanol or butylic fermentation, product reclaim and byproduct comprehensive utilization.In these main production links, biomass pre-treatment is in core status, this is because first biomass pre-treatment has determined the efficiency of cellulase hydrolysis, if without biomass pre-treatment, the enzymatic hydrolyzation of cellulose biomass is generally no more than 30%, and needs a large amount of zymins, by the suitable pre-treatment of intensity, cellulosic enzymatic hydrolyzation can significantly improve, and even can reach 100%.The complicated components of biomass, if one of them component of single utilization, except cause principle utilization ratio lower, the component of not utilizing also causes environmental pollution, therefore the comprehensive utilization of biomass is preconditions that biomass efficient utilizes, and suitable pretreatment process is the essential condition that ensures comprehensive utilization.Therefore, the importance of biomass pre-treatment in biorefinery process is self-evident.
People pay attention to the pretreated importance of biomass very early, have developed various and treatment process.According to current sorting technique, substantially can be divided into physics pre-treatment, Chemical Pretreatment, Biological Pretreatment, in order to overcome the shortcoming of single pretreatment process, bring into play its advantage, also develop the pretreated method of combination.But the value-added effect that corresponding existing biomass utilization produces, the greatest problem of pre existing processing mode is that cost is too high.Easily hundreds of units pre-treatment cost per ton, by advantage approach exhaustion cheap biomass material.The reason that these method costs are higher can be divided into several aspects: the one, need to consume the chemical of some amount, as acid, alkali, ammonia, carbonic acid gas etc., such pretreatment process is in the time solving bad chemical recovery problem, can cause cost to increase sharply, and to solve recovery problem, and just need to invest a certain amount of recovery system, increase facility investment.Second aspect that cost is high is to need high energy consumption, such as hydrothermal pretreatment, dilute acid pretreatment, the high temperature of nearly 200 DEG C need to be provided, by biomass material, be mainly that (hydrothermal pretreatment need to be in liquid-solid ratio up to 10: 1-20: carry out under 1 condition) be heated to 200 DEG C, the energy needing is very high for water in biomass material, if such raw material, for the production of biomass energy, just may cause losing more than gain on the energy.The another one reason that pre-treatment cost is higher is the high-intensity equipment of conditional request of pre-processing device, and such as hydro-thermal, diluted acid all need to carry out under the pressure of tens kilograms, and such pressure causes the strength demand of equipment very high, and cost is higher.
Therefore, exploitation less energy-consumption, low cost, high efficiency pretreatment process, remains the active demand of biorefinery industry.Application number is 200910069710.9 patent of invention, the method of the synchronous coupling process of a kind of microwave-steam explosion to straw removing crystallization disclosed, the method is the heating source for the quick-fried device of vapour by microwave, utilize the quick-fried advantage of microwave and vapour simultaneously, removed and have certain effect for the degree of crystallinity of stalk, still, use in conjunction with the quick-fried device of vapour, still be difficult to avoid the use of high pressure vessel, and cannot produce continuously, efficiency is not high.Application number is that 200710144429.8 Chinese invention patent discloses a kind of raw material microwave pre-treatment method for Production of Fuel Ethanol, the key step of the method be by matrix powder according to solid-to-liquid ratio 1: 30-50 adds water, under microwave condition, process 30-60min, afterwards washing and filtering.Although the method treating processes is comparatively simple, in treating processes, to use a large amount of water, in the time that technical scale is used this method, must cause a large amount of waste water to produce, the use of simultaneously large water gaging, also can cause the energy in heat-processed mainly to be absorbed by water, makes to process energy consumption high.
Summary of the invention
[goal of the invention], although the pretreated method of biomass is varied at present, general problem is that cost is higher.In order to make full use of the cheap advantage of biomass resource, need the pretreatment mode that cost of development is lower, realize the high-valued of biomass.Thereby be real reproducible resource by the Wood Adhesives from Biomass of " need not be rubbish, utilize not worthwhile ".
[design of the present invention] is in order to realize the Efficient Conversion of biomass resource, pre-treatment is essential, why pre-treatment can increase the transformation efficiency of biomass, be commonly considered as working by several aspects: the one, the granularity of biomass is reduced, increase the void volume that cellulase can enter matrix inside; The 2nd, reduce cellulosic degree of crystallinity, increase cellulosic degradability; The 3rd, destroy cellulosic structural barriers by degradation of hemicellulose and xylogen.Different pretreatment processs, often by the various combination of these effects different pretreating effect that is effective.In these pretreatment processs, vapour is quick-fried is a kind of highly versatile, the lower-cost a kind of pretreatment process of pre-treatment, its ultimate principle is to pass through saturation steam at airtight inside reactor, at 200 DEG C, maintain several minutes, then the valve of reactor is opened fast, the material that makes inside reactor is produced fast, thereby complete preprocessing process.From microanalysis, the material of certain water content is under the heating of high-temperature steam, make the moisture gasification in material, form certain vapour pressure, such material is under the condition of quick pressure releasing, the pressure that the cell wall structure of material inside can be fast released breaks through, and reduces material particles degree thereby reach, and increases the effect of material wood interior porosity.Microwave Pretreatment is a kind of research pretreatment process early, be commonly considered as a kind of physical treatment method, mainly by carrying out microwave radiation to material, make material be issued to higher temperature at airtight container, microwave treatment also has strong effect to the structure of cellulosic molecule simultaneously, can reduce cellulosic degree of crystallinity, increase cellulosic degradability.The higher liquid-solid ratio of the general use of Microwave Pretreatment, higher pressure, this just causes the cost of reactor higher (need to make pressure vessel), produce a large amount of organic waste water (Mierocrystalline cellulose of Partial digestion can be dissolved in water), energy consumption higher (will heat a large amount of water).But microwave has unique advantage, its homogeneous heating, speed, can receive soon soon send out.Therefore microwave is also had to unique advantage as a kind of type of heating.
The pretreated important effect source of biomass is exactly temperature, in the time that material is processed in non-encloses container, in the time that water-content is higher, the temperature of material can not reach more than 100 DEG C, in order to reach higher temperature, comparatively normal method adopting be exactly by streams closed among container, then microwave is imported in container and is heated to material, at this moment temperature of charge can reach the high temperature of 200 DEG C.When the water content of material hour, carry out microwave heating to material, will make the temperature of material sharply raise, even can make material carbonization, have human hair to understand the method for with microwave, material carbonization being produced to gac.In the time that material is carried out to microwave radiation, the water in material is the best medium of microwave energy absorbing, and therefore the moisture in material is the important factor that determines heating material effect.Consider biomass material, especially cellulose biomass is the cell walls of plant substantially, if absorbed in material after portion of water, will have moisture to arrive the inside of cell walls.If give this part moisture rapid heating, completely likely make this part moisture gasification, in the time that the moisture of gasification cannot rapid osmotic goes out cell walls, just likely accumulate certain pressure, and then cell walls is burst, and then the temperature of biomass is elevated to and exceedes 100 DEG C of above high temperature, and without the reactor by airtight.So just using each cellularstructure of cellulose biomass as a quick-fried reactor of miniature vapour.In order to realize this imagination, need the several preconditions that meet to be, the moisture content in material is suitable, and the speed that moisture becomes gaseous state from liquid state will reach certain requirement.Based on above imagination, on the basis of repetition test, the present invention is proposed.
[technical solution of the present invention] essential characteristic of the present invention is as follows:
(1) first biomass material to be processed need is cut off and pulverization process, make its granularity scope between 1-50mm, raw material is comparatively even like this, is convenient to moisture controlled and homogeneous heating; (2) then according to the water-content of raw material, spray tap water to biomass, regulate its water content to 10-30% (mass ratio), be uniformly distributed in the requirement of cell interior in order to reach water content, after spraying tap water, uniformly mixing raw material, and standing 1-24h, make moisture evenly infiltrate material inside; (3) after the material metage after water balance, put into microwave reactor and process, initial adjustment unit mass microwave irradiation power between 50-1000w/kg wet stock, preheating material, be 1-10min warm up time; (4) when the temperature of material reaches after 95 DEG C-98 DEG C, regulate microwave irradiation power between 1-5kW/kg wet stock, moisture in Quick-gasifying material, under Quick-gasifying condition, water vapour expands and does work, the cell walls of biomass material is destroyed, and then increase specific surface area and the porosity of material.At this moment temperature of charge is elevated to 130-150 DEG C, keeps with this understanding 10-1000s to complete primary treatment.The feature of whole preprocessing process is by control moisture, and low power heating in the early stage improves temperature, and moisture is uniformly distributed, and later stage rapid heating makes moisture Quick-gasifying, at inner microcosmic explosion, degradation of hemicellulose, the porosity of increase raw material of forming of biomass.According to the difference of biomass material and pre-treatment object, can re-treatment step (2) arrive (4) 1 times to 3 times, increase the intensity of processing.
Described biomass material is maize straw, rice straw, wheat stalk, beanstalk, Chinese sorghum, the agricultural crop straws such as sweet sorghum; Clover, the herbaceous plant such as hybrid giant napier; Wood shavings, the each several part of the xylophytas such as twig; The each several part of Chinese silvergrass, switchgrass, fast-growing willow equal energy source plant.
Pre-treatment object comprises produces sugar by pretreated raw material for enzymolysis, by pretreated raw material for the production of alcohol fuel, butanols, the liquid fuels such as succinic acid or Chemicals, pretreated raw material is used for to solid-state fermentation substrate, pretreated raw material, for the production of animal-feed, is used for to anaerobically fermenting by pretreated matrix.
The present invention has following characteristics and advantage:
1. this pre-treatment belongs to dry method or semidrying pre-treatment, although there is certain water content in treating processes in material, but there is no free-water, treating processes can be evaporated portion of water, after finishing dealing with, the content of moisture is 8%-20% (mass ratio), there is no contaminated wastewater, and such material is in the time of the follow-up conversion process for such as enzymatic hydrolysis and fermentation, be conducive to improve material concentration, and then improve product concentration;
2. this pre-treatment is carried out under normal pressure, and the benefit of bringing is like this, has reduced the investment of equipment, has saved in preprocessing process and has feeded, and the process of discharging, has saved the treatment time, has increased processing efficiency, and is convenient to the continuous operation of pretreatment reaction device;
3. because treating processes is carried out under compared with low water content condition, without moisture is carried out to extra heating, thereby reduced processing energy consumption;
In treating processes without adding the chemical such as soda acid, avoided pollution, effectively reduce pre-treatment cost.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
Dry microwave or semidrying pre-treatment maize straw are for enzymatic hydrolysis and fermentation production of cellulosic ethanol.
Within 2010, be harvested from Guan County, Hebei province maize straw first pulverize with plant pulverizer, after pulverizing, cross the sieve of 1mm, take 100g as the pretreated raw material of dry microwave.Measure the water content in stalk, according to lacked amount, spray into tap water, the water content in stalk is adjusted to 30%, stir, be placed in 2L beaker, with preservative film, beaker mouth is sealed up to rear hold over night, make moisture evenly penetrate into material inside.Sample after water balance being put into the household microwave oven of capable of regulating power processes, in treating processes, use a temperature of having wrapped up the Pt100 temperature sensor monitors material of tetrafluoroethylene, first heating power is adjusted to 100w, processes after 5min, temperature reaches 95 DEG C.Then the heating power of microwave oven is adjusted to 500w, carries out rapid heating, at this moment temperature fast rise, reaches rapidly 137 DEG C, processes with this understanding 100s and completes preprocessing process 1 time.Material after finishing dealing with, water content has been reduced to 20%, has a kind of fragrance of maize straw, and has no irritating odor, and color deepens a little.Utilize x-ray diffraction method to measure the Mierocrystalline cellulose percent crystallization in massecuite of the sample of pre-treatment front and back, result shows that dry microwave pre-treatment has reduced by 13.5% by cellulosic percent crystallization in massecuite.Pre-treatment cost has been carried out to comprehensive accounting, and result is 56 yuan of stalks per ton, and with respect to other pretreatment processs, cost significantly reduces.
Pretreated raw material adds after 20IU cellulase/g Mierocrystalline cellulose in proportion for cellulosic enzymolysis, and after enzymolysis 48h, cellulosic enzymatic hydrolyzation is 85%.The corresponding maize straw without microwave treatment, its enzymatic hydrolyzation only has 25%.
Embodiment 2
Dry microwave or semidrying pre-treatment wheat stalk are for solid state fermentation raw material.
First the wheat stalk that is harvested from Beijing for 2010 is pulverized with plant pulverizer, crosses the sieve of 2mm after pulverizing, and takes 200g as the pretreated raw material of dry microwave.Measure the water content in stalk, according to lacked amount, spray into tap water, the water content in stalk is adjusted to 25%, stir, be placed in 3L Glass Containers, with preservative film, beaker mouth is sealed up to rear hold over night, make moisture evenly penetrate into material inside.Sample after water balance being put into the microwave reactor of capable of regulating power processes, in treating processes, use a temperature of having wrapped up the Pt100 temperature sensor monitors material of tetrafluoroethylene, first heating power is adjusted to 150w, processes after 5min, temperature reaches 95 DEG C.Then the heating power of microwave reactor is adjusted to 1000w, carries out rapid heating, at this moment temperature fast rise, reaches rapidly 130 DEG C, processes with this understanding 20s and completes preprocessing process 1 time.Same method carries out primary treatment again.Material after finishing dealing with, water content has been reduced to 18%, has no irritating odor, and color deepens a little.Utilize x-ray diffraction method to measure the Mierocrystalline cellulose percent crystallization in massecuite of the sample of pre-treatment front and back, result shows that dry microwave pre-treatment has reduced by 12.3% by cellulosic percent crystallization in massecuite.
Pretreated raw material carries out viride solid state fermentation as the culture medium of cellulase.Raw material after treatment and wheat bran are according to carrying out proportioning at 4: 1, add the inorganic salt solution (ammonium sulfate 6% (w/w) of 1: 2.5 (w/w), magnesium sulfate 3% (w/w), dipotassium hydrogen phosphate 1.5% (w/w)), at 121 DEG C, carry out after sterilizing 30min, cooling, the viride seed liquor of inoculating 1: 0.5 (w/v) is fermented, temperature is 30 DEG C, ferment after 5 days, enzyme is lived as 65IU/g dry medium, considerably beyond contrast (untreated) 12IU/g dry medium.
Embodiment 3
Dry microwave or semidrying pretreated water rice straw are for biogas fermentation material.
First the rice straw that is harvested from Liaoning for 2010 is pulverized with plant pulverizer, crosses the sieve of 5mm after pulverizing, and takes 100g as the pretreated raw material of dry microwave.Measure the water content in stalk, according to lacked amount, spray into tap water, the water content in stalk is adjusted to 20%, stir, be placed in 2L Glass Containers, with preservative film, beaker mouth is sealed up to rear hold over night, make moisture evenly penetrate into material inside.Sample after water balance being put into the microwave reactor of capable of regulating power processes, in treating processes, use a temperature of having wrapped up the Pt100 temperature sensor monitors material of tetrafluoroethylene, first heating power is adjusted to 50w, processes after 5min, temperature reaches 95 DEG C.Then the heating power of microwave reactor is adjusted to 1000w, carries out rapid heating, at this moment temperature fast rise, reaches rapidly 132 DEG C, processes with this understanding 30s and completes preprocessing process 1 time.Same method carries out twice processing again.Material after finishing dealing with, water content has been reduced to 15%, has no irritating odor, and darkens.Utilize x-ray diffraction method to measure the Mierocrystalline cellulose percent crystallization in massecuite of the sample of pre-treatment front and back, result shows that dry microwave pre-treatment has reduced by 12.7% by cellulosic percent crystallization in massecuite.
These materials, for biogas fermentation, adopt 1L wide-necked bottle as reactor, and material gross weight is 500g, and total solids (TS) concentration is 6%, and inoculum density is 45%, and fermentation period is 50d, and two of experiment employings are parallel, and one is experiment sample, and one is control sample.When experiment starts, in reactor, be filled with nitrogen 3min guarantee anaerobic environment.By rubber stopper seal, put into the incubator of 35 degrees Celsius and cultivate, adopt drainage to collect biogas, Timing measurement biogas output.Experimental result shows: 30d arrives aerogenesis peak, and gas production rate is 926ml, and methane content is 67.8%; Cumulative gas production is 11001ml, and the TS of unit gas production rate is 366.7ml/g; And the not pretreated control group of rice straw arrives aerogenesis peak 598ml to 40d, methane content is 60.1%, cumulative gas production 9211ml, and the TS of unit output is 307ml/g, all lower than pretreated raw material.
Claims (3)
1. a method for dry microwave or semidrying preprocessing biomass, is characterized in that: (1) first cuts off biomass material to be processed need and pulverization process, makes its granularity scope between 1-50mm; (2) then according to the water-content of raw material, spray tap water to biomass, regulate its water content to 10-30%(w/w), uniformly mixing raw material, and standing 1-24h, make moisture evenly infiltrate material inside; (3) after the material metage after water balance, put into microwave heating installation and process, initial adjustment unit mass microwave irradiation power between 50-1000w/kg wet stock, preheating material, be 1-10min warm up time; (4) when the temperature of material reaches after 95 DEG C-98 DEG C, regulate microwave irradiation power between 1-5kW/kg wet stock, temperature of charge is elevated to 130-150 DEG C, keeps with this understanding 10-1000s to complete primary treatment; According to the difference of biomass material and pre-treatment object, can re-treatment step (2) arrive (4) 1 times to 3 times, increase the intensity of processing.
2. method according to claim 1, is characterized in that: described biomass are corn, paddy rice, wheat, beanstalk, Chinese sorghum, the stalk of sweet sorghum; Clover, hybrid giant napier; Wood shavings, twig; The each several part of energy-source plant Chinese silvergrass, switchgrass, fast-growing willow.
3. method according to claim 1, it is characterized in that: described pre-treatment object comprises produces sugar by pretreated raw material for enzymolysis, by pretreated raw material for the production of alcohol fuel, butanols, succinic acid, pretreated raw material, for solid-state fermentation substrate, for the production of animal-feed, is used for to anaerobically fermenting by pretreated matrix by pretreated raw material.
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| WO2018145297A1 (en) * | 2017-02-10 | 2018-08-16 | 江苏京海禽业集团有限公司 | Preparation method for straw feed and biological straw feed |
| CN110791540A (en) * | 2019-11-08 | 2020-02-14 | 孟保奎 | Method for quickly pretreating biomass by microwave alkaline baking |
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