CN102660587A - Method for pretreating lignocellulose raw material continuously/intermittently under normal pressure by using calcium chloride solution - Google Patents
Method for pretreating lignocellulose raw material continuously/intermittently under normal pressure by using calcium chloride solution Download PDFInfo
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Abstract
The invention discloses a method for pretreating lignocellulose raw material continuously/intermittently under normal pressure by using a calcium chloride solution. The method comprises the following steps: (1) carrying out crashing, washing and impurity removing on the raw material; (2) adding the calcium chloride solution with the concentration of 40 to 70% (m/m) into the raw material to mix; (3) sending the mixed material into a microwave reactor to heat; (4) washing after treatment is finished, and obtaining a solid rich in cellulose and lignin and an xylose solution through solid-liquid separation; and (5) dehydrating the calcium chloride solution, recycling dehydrated water to the step (4), and recycling the calcium chloride concentrate to the step (2). High temperature needed by the pretreatment can be obtained under normal pressure, so that a high-pressure container is omitted, meanwhile, the continuous operation during the treatment process is convenient to realize, the stability of the pretreatment condition is ensured, the comprehensive utilization of three components of lignocellulose is realized technically, and no waste water is produced.
Description
Technical field
The invention belongs to biomass preconditioning technique field, particularly a kind of calcium chloride solution normal pressure method of preprocessing lignocellulose raw material continuously/intermittently of utilizing.
Background technology
Exhaustion day by day along with the petrochemical industry resource; Substitute the petrochemical industry resource with reproducible biomass resource; Is biomass energy through the biorefinery technology with Wood Adhesives from Biomass; Biomass chemical and biological material are developing direction from now on, also are to solve the inevitable means of human environment, resource and energy problem from now on.Biorefinery is an example with the production of bioenergy, and its basic procedure is: biomass collection, biomass pre-treatment, cellulase hydrolysis, ethanol or butylic fermentation, product reclaim and the sub product comprehensive utilization.In these several main production links, the biomass pre-treatment is in core status, and this is because the biomass pre-treatment has at first determined the efficient of cellulase hydrolysis; If without the biomass pre-treatment; The enzymatic hydrolyzation of cellulose biomass generally is no more than 30%, and needs a large amount of zymins, through the intensity appropriate pretreatment; Cellulosic enzymatic hydrolyzation can significantly improve, even can reach 100%.The component of biomass is complicated; If one of them component of single utilization; Except causing the principle utilization ratio than low; The component of utilizing does not also cause environmental pollution, so the comprehensive utilization of biomass is preconditions that biomass efficient utilizes, and suitable pretreatment process is the essential condition that guarantees comprehensive utilization.Therefore, the importance of biomass pre-treatment in the biorefinery process is self-evident.
People pay attention to the pretreated importance of biomass very early, have developed various pretreatment processs.According to present sorting technique, can be divided into physics pre-treatment, Chemical Pretreatment, Biological Pretreatment basically, in order to overcome the shortcoming of single pretreatment process, bring into play its advantage, also developed the pretreated method of combination.But the value-added effect that corresponding existing biomass utilization is produced, the greatest problem of pre existing processing mode is that cost is too high.Easily the pre-treatment cost that hundreds of units are per ton, the advantage approach exhaustion that biomass material is cheap.The higher reason of these method costs can be divided into several aspects: the one, need to consume the chemical of some amount, and like acid, alkali; Ammonia, carbonic acid gas etc., such pretreatment process is when solving bad chemical recovery problem; Can cause cost to increase sharply; And to solve the recovery problem, and just need a certain amount of recovery system of investment, increase facility investment.Second aspect that cost is high is to need high energy consumption, such as hydrothermal pretreatment, and dilute acid pretreatment; Nearly 200 ℃ high temperature need be provided; With biomass material, mainly be that the water (hydrothermal pretreatment need be carried out under up to the condition of 10:1-20:1 in liquid-solid ratio) in the biomass material is heated to 200 ℃, the energy that needs is very high; If such raw material is used for the production of biomass energy, just possibly cause losing more than gain on the energy.The higher another one reason of pre-treatment cost is the high-intensity equipment of conditional request of pre-processing device, and such as hydro-thermal, diluted acid all need carry out under tens kilograms pressure, and such pressure causes the strength demand of equipment very high, and cost is higher.
Therefore, the 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, discloses the method for the synchronous coupling process of a kind of microwave-steam explosion to the straw removing crystallization, and this method is used for microwave the heating source of the quick-fried device of vapour; Utilized the quick-fried advantage of microwave and vapour simultaneously, removing for the percent crystallinity of stalk has certain effect, still; Use in conjunction with the quick-fried device of vapour; Still be difficult to avoid the use of high pressure vessel, and can't continuous production, efficient is not high.Application number is that 200710144429.8 Chinese invention patent discloses a kind of raw material microwave pre-treatment method that is used for Production of Fuel Ethanol; The key step of this method is that the matrix powder is added entry according to solid-to-liquid ratio 1:30-50; Under microwave condition, handle 30-60min, washing and filtering afterwards.Though this method treating processes is comparatively simple, will use a large amount of water in the treating processes, when technical scale is used this method; Must cause great amount of wastewater to produce; The use of simultaneously big water gaging also can cause the energy in the heat-processed mainly to be absorbed by water, makes the processing energy consumption high.
Summary of the invention
[goal of the invention] though 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 lower pretreatment mode of cost of development, realize the high-valued of biomass.Thereby with the Wood Adhesives from Biomass of " need not be rubbish, utilize not worthwhile " is real reproducible resource.
[design of the present invention] high temperature in order to realize that pre-treatment is required; Avoid the use of pressurized vessel simultaneously, people such as Kitchaiya (Intanakul, P.; Krairiksh; M., Kitchaiya, P.2003.Enhancement of enzymatic hydrolysis of lignocellulosic wastes by microwave pretreatment under atmospheric pressure.J.Wood Chem.Technol.23; 217-225.) reported and used the microwave absorbing medium of glycerine as the Microwave Pretreatment process, and obtained good effect.Pretreated temperature can reach 200 degrees centigrade in this medium.Use the higher comparatively cheap raw material of organic solvent pre-treatment of price, pretreated cost is increased.People (Tokuyasu, K., Tabuse such as nearest Tokuyasu; M., Miyamoto, M.; Matsuki, J., Yoza; K.2008.Pretreatment of microcrystalline cellulose flakes with CaCl2increases the surface area, and thus improves enzymatic saccharification.Carbohydr.Res.343 1232-1236.) has reported with calcium chloride solution and has soaked Microcrystalline Cellulose at normal temperatures as a kind of pretreatment mode; Though this pretreatment mode have effect preferably for microcrystalline cellulose,, but there is not effect basically for natural xylogen raw material.Make full use of the high boiling point of calcium chloride solution, utilize the effect of calcium chloride solution simultaneously,, can under normal pressure, realize the high processing temperature like this, thereby realize pretreating effect preferably with microwave heating source the most for Mierocrystalline cellulose polymer crystallization hydrogen bond.
[technical scheme of the present invention] essential characteristic of the present invention is following:
(1) at first lignocellulosic material is crushed to the particle of 1-20mm with kibbler, the impurity such as sandstone in the raw material are removed in washing; (2) adding concentration according to solid-to-liquid ratio 1:5-15 (m/v) is the calcium chloride solution of 40-70% (m/m), mixes; (3) the material continuously feeding that mixes is sent into continuously/carry out microwave heating in the batch microwave reactor drum, regulating power, to make the material temperature scope be 140-180 ℃, and regulating input speed, to make the residence time of material in reactor drum be 5-15min; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool; The solid substance that obtains rich cellulose and xylogen after the solid-liquid separation can be used for the subsequent technique of biorefinery; Liquid portion after the solid-liquid separation is through the ion exchange column decolouring; Obtain wood sugar liquid after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through high-efficiency evaporator, the water that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator that obtains is back to process step (2).
The present invention has following characteristics and advantage:
1. calcium chloride solution is used for the pre-treatment of lignocellulosic material, under normal pressure, can obtains the required high temperature of pre-treatment, thereby avoided the use of high pressure vessel, also be convenient to realize simultaneously the continuous operation of treating processes, guarantee the stability of pretreatment condition;
2. calcium chloride is used for pre-treatment repeatedly through the reuse process; Reduced the pre-treatment cost; Because calcium chloride is nontoxic; Little to environmental hazard, can follow-up enzymatic hydrolysis and fermentation not impacted even flow into downstream process on a small quantity yet, growth and the ethanol fermentation to yeast cell has certain promoter action on the contrary;
3. pretreatment technology fully takes into account xylogen, and the comprehensive utilization of Mierocrystalline cellulose and semicellulose has not only obtained being easy to the solid substance (mainly comprising Mierocrystalline cellulose and xylogen) of enzymatic hydrolysis and fermentation in the preprocessing process, also obtained wood sugar;
4. the abundant reuse of process water, no waste water produces.
Description of drawings
Fig. 1 utilizes the calcium chloride solution normal pressure process flow sheet of preprocessing lignocellulose raw material continuously/intermittently;
1, lignocellulosic material; 2, the solid substance of rich cellulose and xylogen; 3, wood sugar; 4, calcium chloride solution; 5, water; 6, kibbler; 7, washing pool; 8, stirred pot; 9, continuously/the intermittent type microwave reactor drum; 10, washing pool; 11, suction filtration/whizzer/spiral is extracted machine; 12, ion exchange column; 13, high-efficiency evaporator.
Embodiment
Through embodiment the present invention is further specified below, but be not used in the claim scope of the present invention that limits.
Utilize method pre-treatment corn straw of the present invention.
(1) at first corn straw is crushed to the particle of 2mm with RT-34S type kibbler, the impurity such as sandstone in the raw material are removed in washing; (2) in 100g corn straw (dry weight), adding concentration according to solid-to-liquid ratio 1:10 (m/v) is the calcium chloride solution 1000mL of 62.5% (m/m), mixes; (3) place the MR-3 microwave reactor to carry out microwave heating the material that mixes, it is 160 ℃ that adjusting power makes material temperature, and the treatment time is 10min; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool; Obtain the solid substance (70g of rich cellulose and xylogen after the solid-liquid separation; Dry weight) can be used for enzymolysis malaga sugar; Liquid portion after the solid-liquid separation obtains wood sugar liquid through the ion exchange column decolouring after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through Rotary Evaporators, the water that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator that obtains is back to process step (2).
The solid substance that obtains has been measured its specific surface area, and the result is 2.77m
2/ g, the value of handling raw material has increased by 189%.Measured its crystallinity index, the result shows, has reduced by 13.9%.Pretreated raw material has been carried out the enzymolysis experiment, and cellulosic enzymatic hydrolyzation is 90.66%, and corn straw and the steam puffed stalk of under similarity condition, thinking processing are as contrast, and cellulosic enzymatic hydrolyzation is 32% and 66% in untreated corn straw and the steam puffed stalk.The result shows that the calcium chloride pre-treatment has effectively increased the specific surface area of corn straw, has reduced its cellulosic crystalline indice, thereby has effectively improved its hydrolysis result.
Utilize method pre-treatment corn straw of the present invention.
(1) at first corn straw is crushed to the particle of 20mm with RT-34S type kibbler 6, the impurity such as sandstone that washing 7 is removed in the raw materials; (2) in corn straw, add the calcium chloride solution 4 that concentration is 40% (m/m) according to solid-to-liquid ratio 1:15 (m/v), mix 8 even; (3) place module manifold type biomass microwave dry method or the continuous pretreatment reaction device 9 of semidrying (number of patent application 201110163346.X) to carry out microwave heating the material that mixes; It is 140 ℃ that adjusting power makes the material temperature scope, and it is 15min that the adjusting input speed makes the residence time of material in reactor drum; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool 10; Use spiral to extract the substrate that the solid substance 2 that obtains rich cellulose and xylogen after machine 11 solid-liquid separation can be used for solid state fermentation; Liquid portion after the solid-liquid separation is through the ion exchange column decolouring; Obtain wood sugar liquid 3 after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through triple effect evaporation 13, the water 5 that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator 4 that obtains is back to process step (2).
Utilize method pre-treatment wheat stalk of the present invention.
(1) at first wheat stalk is crushed to the particle of 10mm with RT-34S type kibbler 6, the impurity such as sandstone that washing 7 is removed in the raw materials; (2) in corn straw, add the calcium chloride solution 4 that concentration is 60% (m/m) according to solid-to-liquid ratio 1:5 (m/v), mix 8 even; (3) place module manifold type biomass microwave dry method or the continuous pretreatment reaction device 9 of semidrying (number of patent application 201110163346.X) to carry out microwave heating the material that mixes; It is 170 ℃ that adjusting power makes the material temperature scope, and it is 12min that the adjusting input speed makes the residence time of material in reactor drum; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool 10; Use spiral to extract the substrate that the solid substance 2 that obtains rich cellulose and xylogen after machine 11 solid-liquid separation can be used for solid state fermentation; Liquid portion after the solid-liquid separation is through the ion exchange column decolouring; Obtain wood sugar liquid 3 after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through triple effect evaporation 13, the water 5 that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator 4 that obtains is back to process step (2).
Utilize method pretreated water rice straw of the present invention.
(1) at first rice straw is crushed to the particle of 1mm with RT-34S type kibbler 6, the impurity such as sandstone that washing 7 is removed in the raw materials; (2) in corn straw, add the calcium chloride solution 4 that concentration is 65% (m/m) according to solid-to-liquid ratio 1:10 (m/v), mix 8 even; (3) place module manifold type biomass microwave dry method or the continuous pretreatment reaction device 9 of semidrying (number of patent application 201110163346.X) to carry out microwave heating the material that mixes; It is 162 ℃ that adjusting power makes the material temperature scope, and it is 9min that the adjusting input speed makes the residence time of material in reactor drum; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool 10; Use spiral to extract the substrate that the solid substance 2 that obtains rich cellulose and xylogen after machine 11 solid-liquid separation can be used for solid state fermentation; Liquid portion after the solid-liquid separation is through the ion exchange column decolouring; Obtain wood sugar liquid 3 after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through triple effect evaporation 13, the water 5 that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator 4 that obtains is back to process step (2).
Claims (2)
1. one kind is utilized the calcium chloride solution normal pressure method of preprocessing lignocellulose raw material continuously/intermittently; It is characterized in that; Its step and condition are following: (1) at first is crushed to the particle of 1-20mm with lignocellulosic material with kibbler, and the impurity such as sandstone in the raw material are removed in washing; (2) adding concentration according to solid-to-liquid ratio 1:5-15 (m/v) is the calcium chloride solution of 40-70% (m/m), mixes; (3) material that mixes is sent into continuously carried out microwave heating in the intermittence/continuous microwave reactor drum, regulating power, to make the material temperature scope be 140-180 ℃, and regulating input speed, to make the residence time of material in reactor drum be 5-15min; (4) material after finishing dealing with adds washing and removes calcium chloride in washing pool; The solid substance that obtains rich cellulose and xylogen after the solid-liquid separation can be used for the subsequent technique of biorefinery; Liquid portion after the solid-liquid separation is through the ion exchange column decolouring; Obtain wood sugar liquid after the desalination, can be used for xylose crystalline; (5) extract calcium chloride dilute solution behind the wood sugar and dewater concentratedly through high-efficiency evaporator, the water that removes is back to the washing in (4) step, and the calcium chloride liquid concentrator that obtains is back to process step (2).
2. a kind of calcium chloride solution normal pressure method of preprocessing lignocellulose raw material continuously/intermittently of utilizing according to claim 1; It is characterized in that described lignocellulosic material is meant various shells, hardwood, cork, various agricultural crop straw and Chinese silvergrass, the living willow of speed, the living poplar of speed, the paper mulberry equal energy source plant that contains xylogen.
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Cited By (4)
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| CN102977058A (en) * | 2012-12-07 | 2013-03-20 | 中国科学院过程工程研究所 | Method for producing furfural |
| CN105505993A (en) * | 2014-09-24 | 2016-04-20 | 北京大学深圳研究生院 | Combined pre-treatment method of cellulose-type biomass for biologically producing hydrogen |
| CN112111117A (en) * | 2020-10-12 | 2020-12-22 | 新疆农业大学 | Environment-friendly wood-plastic composite material treated by microorganisms, and preparation method and application thereof |
| CN112143835A (en) * | 2020-08-25 | 2020-12-29 | 长春欣瑞德新材料科技开发有限公司 | Method for extracting multiple polysaccharide substances from biomass material |
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Cited By (4)
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| CN102977058A (en) * | 2012-12-07 | 2013-03-20 | 中国科学院过程工程研究所 | Method for producing furfural |
| CN105505993A (en) * | 2014-09-24 | 2016-04-20 | 北京大学深圳研究生院 | Combined pre-treatment method of cellulose-type biomass for biologically producing hydrogen |
| CN112143835A (en) * | 2020-08-25 | 2020-12-29 | 长春欣瑞德新材料科技开发有限公司 | Method for extracting multiple polysaccharide substances from biomass material |
| CN112111117A (en) * | 2020-10-12 | 2020-12-22 | 新疆农业大学 | Environment-friendly wood-plastic composite material treated by microorganisms, and preparation method and application thereof |
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Application publication date: 20120912 |