CN101092435B - Technical method for separating organic constituent of biomass - Google Patents
Technical method for separating organic constituent of biomass Download PDFInfo
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Abstract
This invention discloses a method for separating biomass organic components. The method comprises: washing classified raw materials, decomposing in a high-pressure reactor under the actions of microwave and ultrasonic wave, and extracting organic components from biomass with 20-70 vol. % aqueous solution of an organic solvent. The separation process comprises: (1) extracting low-temperature-soluble organic component from biomass at 40-120 deg.C under 0.4-0.6 MPa; (2) separating cellulose pulp at 160-220 deg.C; (3) separating acetic acid, lignin and furfural from the liquid (separated by solid-liquid separation) by centrifuge and precipitation. According to different plants, the powers and frequencies of microwave and ultrasonic wave, as well as the reaction temperature and time can be adjusted. The method has such advantages as low organic molecule loss, little change, no harm of the products, high cellulose purity (higher than 95%), low lignin residue (not higher than 2%), and no environmental pollution.
Description
Technical field
The present invention relates to a kind of separating process of organic constituent of biomass.
Background technology
Along with contradiction between oil supply and demand increasingly sharpens, resource is more and more nervous, utilizes biomass resource inexhaustible, nexhaustible on the earth, develops the biomass industry, becomes the inexorable trend of Sustainable development.Biomass are mainly used in burning, generating, liquefaction, gasification etc. as the energy at present, also are used for aspects such as pulping and paper-making, furniture and use, and usage ratio such as pulping and paper-making, viscose fiber, fermentation system ethanol are bigger, and are higher to the biomass processes processing requirement.Mierocrystalline cellulose mainly is made up of plant, be mainly used to produce paper pulp, purified pulp, existing production technique, raw material availability is low, and cause water pollution, topsoil etc. to destroy the serious consequence of environment, but the social demand amount strengthens day by day, and the urban plant waste is well utilization not, can only landfill or combustion power generation, the utility value form is very low, can only how effectively to make full use of plant and biomass resource, but production technology is proposed higher requirement.Shortcomings such as the organic solvent method treatment process is a novel method, and effectively separation and Extraction is utilized plant, but many shortcomings are also arranged, and it is strong to have material choice, and a lot of plants can not be suitable for, and different plant difference on effect is big, and xylogen is residual many, and the separating reaction time is long.
At present, in the lot of domestic and foreign plant treatment technology, all with the chemical acid alkali method, the physics blasting procedure, modes such as biological enzyme are not only polluted big, the power consumption water consumption is many, and plant fails to make full use of, pollution level differs, and is expensive, is difficult to carry out on market, and the raw material limitation is big, can only adopt single or less floristics, the cellulose pulp quality is low, can only satisfy the requirement of paper pulp, or even can only be used to produce low-grade paper pulp, its technological effect is only to get a bit, abandons all the other, makes a lot of organic component wastes, occur with pollution form, factory can only drop into the pollution treatment project again, and cost improves, and midget plant can't be born.Part novel process limitation is too big, also is difficult to promote, and the cellulose pulp of being produced does not reach the requirement of purified pulp substantially; And can reach the technology of purified pulp standard, but its operating procedure complexity, productive rate is low, and cost is very high and seriously polluted.Extremely incompatible with the human environment development trend.
Summary of the invention
The object of the present invention is to provide a kind of separating process of organic constituent of biomass.It is short that this method is separated the time of organic composition, the purity height of isolated organic composition, and this processing method is pollution-free, help environmental protection.
For achieving the above object, the present invention takes following technical scheme:
A kind of separating process of organic constituent of biomass, this method comprises the steps:
(1), be raw material with biomass, and pulverize, with the aqueous solutions of organic solvent infiltration of 20%～70% volumetric concentration, be microwave treatment 5～30min of 700W～5000W with frequency 900MHz～2500MHz, power; The aqueous solutions of organic solvent that adds 20 volume %～70 volume % concentration again, make the biomass particle immerse in the aqueous solutions of organic solvent fully, at 40～120 ℃, pressure is under 0.4MPa～0.6MPa condition, be 15KHz～2.4MHz with frequency again, power is that ultrasonic wave and the frequency of 200W～5000W is 900MHz～2500MHz, power is the microwave of 700W～5000W, handle 5～30min simultaneously, filtering separation then, wherein, biomass are unit with g, aqueous solutions of organic solvent is unit with L, and the volumetrical ratio of the weight of biomass starting material and above-mentioned twice total consumption of aqueous solutions of organic solvent is 500～1000: 0.8～3;
(2), the solid that filtering separation in the step (1) is obtained adds in the aqueous solutions of organic solvent of 20%～70% volumetric concentration, wherein, the solid that filtering separation obtains is unit with g, aqueous solutions of organic solvent is unit with L, and the solid weight that filtering separation obtains and the volumetrical ratio of aqueous solutions of organic solvent consumption are 500～1000: 0.8～3; At 160～220 ℃, pressure is under 1.2MPa～2.6MPa condition, with the frequency is that 15KHz～2.4MHz, power are the ultrasonic wave of 200W～5000W, frequency is that 900MHz～2500MHz, power are that the microwave of 900W～5000W is handled 5～30min simultaneously, carry out solid-liquid separation, the solids that obtains is a Mierocrystalline cellulose;
(3), the liquid after the solid-liquid separation, when cooling 60 ℃～normal temperature, produce the xylogen throw out, the xylogen throw out is through centrifugal treating, it is the xylogen finished product that its solids and pure water mix the solids that obtains after filtering again.
The reaction mechanism of processing method of the present invention is: ultrasonic wave produces the intense impact vibration in reaction solution (being the mixing liquid of biomass particle and aqueous solutions of organic solvent), and plays stirring action, makes H
2O isolates more H
+And OH
-Radical promotes to combine with organic molecule, with other component separating that is attached on the Mierocrystalline cellulose, makes that organic molecule to be dissolved in the liquid.Be raising speed, ultrasonic frequency can adopt the multifrequency mode, generally adopts 15KHz, 20KHz, 50KHz, 100KHz, 1.7MHz or 2.4MHz, and and the microwave acting in conjunction, can reach good effect; Component in the biomass causes that under the effect of microwave intensive polarity vibration produces heat energy, thereby causes between organic molecule hydrogen bond lax, and structure breaking has been quickened solvent molecule to the infiltration of matrix and the dissolving of composition to be extracted.Can adopt 2500MHz, 2450MHz, 2000MHz, 1500MHz, 1000MHz, 915MHz, 900MHz microwave action in reaction solution (being the mixing liquid of biomass particle and aqueous solutions of organic solvent).
The separating process of organic constituent of biomass of the present invention in step (3), the liquid after the solid-liquid separation cools 60 ℃ the time, begins to have the xylogen throw out to produce; Along with the reduction of temperature, reduce to 50 ℃, 40 ℃, the xylogen throw out can little by little increase; Until normal temperature, precipitate fully.
In the separating process of organic constituent of biomass of the present invention, described biomass are one or more in roots of plants, stem, leaf part, feces of livestock and poultry and the plant domestic refuse dead meal.Wherein, roots of plants, stem, leaf part be as leaf wood, pine, fast living poplar, bamboo, wheat straw, reed, corn stalk, bagasse, cotton stalk, agricultural crop straw etc.Can both separate above-mentioned biomass material under processing condition of the present invention, the above-mentioned biomass material of different densities all can separate.But the organism purity that the fine biomass material is produced, performance, purposes are all relatively good; And plant rubbish, animal dung are as biomass material, its use, utility value are lower, and organic waste water then can't be used this processing method, therefore, in preferred use roots of plants, stem, the leaf part one or more hereinafter are also referred to as plant material as biomass material.With biomass is raw material, pulverizes to be particle, is also referred to as crushed aggregate of plant.
In the separating process of organic constituent of biomass of the present invention, described biomass material can adopt dissimilar, as roots of plants, stem, the leaf part, several mixing in feces of livestock and poultry and the plant domestic refuse dead meal etc. are used, but preferably adopt wherein a kind of, therefore, before separation of produced, biomass material to be sorted out, like this, can in separation of produced, can adjust microwave and hyperacoustic power and frequency respectively according to dissimilar biomass materials, and control different reaction times and temperature, to reach corresponding target level of product quality.
In the separating process of organic constituent of biomass of the present invention, described aqueous solutions of organic solvent can be alcohols, acids aqueous organic.As methanol aqueous solution, aqueous ethanolic solution, aqueous propanol solution, aqueous formic acid, acetic acid aqueous solution, oxalic acid aqueous solution, the acetylsalicylic acid aqueous solution, aqueous solution of salicylic acid, any one in the ethyl acetate aqueous solution and the aqueous acetone solution.The concentration of aqueous solutions of organic solvent is 20 volume %～70 volume %, selects for use in this scope according to actual needs.In above-mentioned aqueous solutions of organic solvent, because aqueous ethanolic solution is nontoxic, colourless, cost is low, so the preferred alcohol aqueous solution.
In the separating process of organic constituent of biomass of the present invention, in the described step (1), the liquid that filtering separation obtains is at 40～80 ℃, air pressure is to carry out underpressure distillation under 2KPa～10KPa condition, evaporate fully until organic solvent, obtaining organism is the mixture that comprises tannin, pigment, alkaloid, essential oil, pectin.
In the separating process of organic constituent of biomass of the present invention, in the described step (3), the liquid that obtains through centrifugal treating, filtration treatment is sent in the distillation tower and is distilled, and collects acetate, furfural respectively, and resistates is oligose and wood sugar.
In the present invention, employed KHz is 10
3Hz, MHz are 10
6Hz; KPa is 10
3Pa, MPa are 10
6Pa.
Processing method provided by the invention may be summarized to be: clean sorted raw material, in high-pressure reaction vessel, adopt microwave and ultrasonic wave to act on simultaneously, strengthen and decompose, with the aqueous solutions of organic solvent of 20 volume %～70 volume % concentration, decompose and extract component in the plant.Sepn process mainly is divided into three steps, (1), be under 0.4MPa～0.6MPa condition at 40～120 ℃, pressure, low temperature SOF Soluble Organic Fraction in the extraction plant; (2), at 160～220 ℃, pressure is to isolate cellulose pulp under 1.2MPa～2.6MPa condition; (3), [liquid that solid-liquid separation is come out in (2) step is black liquor to black liquor, so be called black liquor] isolate acetate with conventional centrifugal, coprecipitation mode, organic composition such as xylogen, furfural. according to the plant difference, adjust microwave and hyperacoustic power and frequency respectively, and control different reaction times and temperature, to reach corresponding target level of product quality.
Advantage of the present invention is:
Method of the present invention is to adopt the extraction that combines of electromagnetic radiation (being microwave) and high-frequency sasser (being ultrasonic wave), fully act on microwave and hyperacoustic energy in the biomass, make the separating organic matters in the biomass, microwave and ultrasonic wave have played conclusive effect in reaction process, have good adjustable controllability concurrently, can accurately adjust the production desired parameters, the polymerization degree of pulp can be adjusted as required, not only improve and improved speed of response greatly, shortened the time, and made that organic composition separates more thoroughly, purity is higher.Compare with other production technique, have more advance, pioneering.Processing method of the present invention can make the various organic compositions of biomass be fully utilized, and greatly reduces production cost simultaneously.Organic molecule loss in the biomass, change lessly, product does not have harmful chemical, and the Mierocrystalline cellulose purity of extraction reaches more than 95%, and the xylogen residual quantity is no more than 2%.Method of the present invention is free from environmental pollution, helps environmental protection.
Description of drawings
Fig. 1 is the schema of processing method of the present invention.
Embodiment
As raw material,, desanding is sorted out, cleaned to material plant with roots of plants, stem, leaf part, pulverize, become single a kind of crushed aggregate of plant hereinafter referred to as material plant.As shown in Figure 1, crushed aggregate of plant is separated, through following three steps.
First step, the weight of material plant (g) is 500～1000: 0.8～3 with the ratio of aqueous ethanolic solution (L) (its volumetric concentration is 20%～70%).Soak into earlier, under the normal pressure, and with microwave exposure 5～30min, make electromagnetic energy fully act on component in the plant with a spot of aqueous ethanolic solution; Add the capacity aqueous ethanolic solution of being satisfied with said ratio then, make crushed aggregate of plant immerse in the liquid fully, at 40～120 ℃, pressure is under 0.4MPa～0.6MPa condition, ultrasonic wave and 900MHz～2500MHz, power with 15KHz～2.4MHz, 200W～5000W is the microwave acting in conjunction of 700W～5000W again, extract 5～30min simultaneously, filtering separation then, the solid that solid-liquid separation goes out enter the next step reaction and use; The liquid that solid-liquid separation goes out is by underpressure distillation, temperature remains on 40～80 ℃, air pressure is under 2KPa～10KPa condition, evaporate fully until ethanol, obtaining organism is mixtures such as tannin, pigment, alkaloid, essential oil, pectin, because of floristics difference content differs, because do not contain soda acid and metal ion, behind the concise purifying of mode such as extraction, diafiltration, can be used for fields such as spices, seasonings, natural pigment, herbal medicine, makeup; As not extracting, under the pyritous situation, can be hydrolyzed into acetate, furfural etc., its higher value will reduce, and causes the waste of resource.The heat and the ethanol reusable edible of the evaporation of this step are to reduce energy consumption.
Second step, solids after the extraction adds the aqueous ethanolic solution that reclaims, the weight of solids (g) is 500～1000: 0.8～3 with the ratio of aqueous ethanolic solution (L) (volumetric concentration is 20%～70%), with ultrasonic wave 15KHz～2.4MHz, 200W～5000W, microwave 900MHz～2500MHz, 900W～5000W react 5～30min.Temperature remains on 160～220 ℃, and pressure is 1.2MPa～2.6MPa.When reaching 160 ℃, plant lignin, hemicellulose are dissolved in aqueous ethanolic solution in a large number, and Mierocrystalline cellulose does not dissolve, exist with solid-state form, separate more thoroughly when reaching 200 ℃, carry out solid-liquid separation, solids is a Mierocrystalline cellulose, clean by lower concentration, high temperature alcohol vapour, the cellulose pulp purity that obtains is higher, compares with other technology, does not have acid, alkali resistates in this pulp, can adopt multiple simple and easy technology bleaching, as hydrogen peroxide bleaching, ozone etc.The polymerization degree of cellulose pulp can reach necessary requirement by controlled microwave and hyperacoustic power and frequency and reaction times.The Mierocrystalline cellulose that this stage produces can be widely used in papermaking, purified pulp, reach cellulose fuel.
Third step, the liquid after the solid-liquid separation contains acetate, xylogen, furfural, oligose, wood sugar be not because of containing mineral acid, bases chemical, more easily separated, when cooling 60 ℃～normal temperature, a large amount of xylogen precipitations, centrifugal treating repeatedly pure water obtains the finished product than Vinsol after filtering, surplus solution is sent into distillation tower, and it is oligose and wood sugar that the cut of differing temps can be collected acetate, furfural, resistates respectively.Product can be used for chemical industry, food etc.
Embodiment 1 (is raw material with cizu)
Cizu is cleaned the back chopping be the bamboo piece about 1cm * 1cm, thorough drying, the water that will remain on the plant after soon cleaning evaporates; Get 500g, put in the autoclave, adding concentration is the aqueous ethanolic solution 0.5L of 50 volume %, makes its infiltration, under the normal pressure, and with 2450MHz, 750W microwave, heating 5min; The aqueous ethanolic solution 1L that adds 50 volume % again under the 0.5MPa pressure, remains on 60 ℃, uses 50KHz, 300W ultrasonic wave and 2450MHz, 750W microwave again, handles 10min simultaneously.After processing stops, carry out solid-liquid separation by filter screen, the liquid that solid-liquid separation is come out is to contain the aqueous ethanolic solution that extracts composition, this liquid is in the time of 55 ℃, pressure is underpressure distillation under the 7KPa condition, behind volatilization water outlet and the ethanol, gets the 26g jelly, major ingredient is mixtures such as tannin, alkaloid, can adopt conventional extraction, smart/slightly the mode of heating up in a steamer is separated purification; The solids 465g that solid-liquid separation is come out puts into reactor once more, adding 60 ℃, concentration is the aqueous ethanolic solution 2L of 50 volume %, with 50KHz, 500W ultrasonic wave and 2450MHz, 1000W microwave, handle 15min simultaneously after, temperature reaches 190 ℃, pressure reaches 2.2MPa, decompression steam bleeding, filtering separation in the time of 90 ℃, the solid substance that solid-liquid separation is come out is the bamboo cellulose pulp, after 120 ℃ of alcohol steam washings, surveying its polymerization degree is 700～900, and dry back is 242g; After the liquid that solid-liquid separation is come out is cooled to 50 ℃, generation xylogen precipitation, after filtering, whizzer gets xylogen 127g, surplus liquid is through atmospheric distillation tower, to get concentration be 45 volume % acetate, formic acid mixtures 0.06L to cut in the time of 120 ℃, and cut obtains concentration 50 volume % chaff aldehyde 0.12L in the time of 165 ℃.
Embodiment 2 (is raw material with wood)
Pine is cleaned the back chopping for about 0.5cm * 0.5cm * 0.5cm, thorough drying, the water that will remain on the plant after soon cleaning evaporates; Get 500g, put in the autoclave, adding concentration is the aqueous ethanolic solution 0.5L of 50 volume %, makes its infiltration, under the normal pressure, and with 2450MHz, 750W microwave, heating 10min; Adding concentration again is the aqueous ethanolic solution 1L of 50 volume %, 0.5MPa under the pressure, remain on 80 ℃, use 50KHz/800W ultrasonic wave and the acting in conjunction of 2450MHz/750W microwave again, handle 10min simultaneously, after processing stops, carry out solid-liquid separation by filter screen, the liquid that solid-liquid separation is come out is to contain the aqueous ethanolic solution that extracts composition, and this liquid is in the time of 55 ℃, and pressure is underpressure distillation under the 7KPa condition, behind volatilization water outlet and the ethanol, get the 75g jelly, major ingredient is a tannin, alkaloid, turpentine wet goods mixture can adopt conventional extraction, smart/slightly the mode of heating up in a steamer is separated purification; The solids 478g that again solid-liquid separation is come out puts into reactor once more, adding 60 ℃, concentration is the aqueous ethanolic solution 2L of 50 volume %, with 50KHz/1000W ultrasonic wave and the acting in conjunction of 2450MHz/2000W microwave, handle 15min simultaneously after, temperature reaches 200 ℃, pressure reaches 2.6MPa, decompression steam bleeding, filtering separation in the time of 90 ℃, the solid substance that solid-liquid separation is come out is the wood cellulose pulp, after 120 ℃ of alcohol steam washings, surveying its polymerization degree is 600～800, and dry back is 275g; After the liquid that solid-liquid separation is come out is cooled to 50 ℃, generation xylogen precipitation, after filtering, whizzer gets xylogen 118g, surplus liquid is through atmospheric distillation tower, to get concentration be 35 volume % acetate, formic acid mixtures 0.03L to cut in the time of 120 ℃, and cut obtains concentration 50 volume % chaff aldehyde 0.05L in the time of 165 ℃.
Embodiment 3 (is raw material with the corn stalk)
Corn stalk is cleaned the back chopping for about 2cm * 2cm, and thorough drying is got 500g, puts in the autoclave, and adding concentration is the aqueous ethanolic solution 0.5L of 50 volume %, makes its infiltration, under the normal pressure, and with 2450MHz microwave 750W, heating 5min; Adding concentration again is the aqueous ethanolic solution 1L of 50 volume %, 0.5MPa under the pressure, remain on 60 ℃, use 50KHz, 500W ultrasonic wave and the acting in conjunction of 2450MHz/750W microwave again, handle 5min simultaneously, after processing stops, carry out solid-liquid separation by filter screen, the liquid that solid-liquid separation is come out is to contain the aqueous ethanolic solution that extracts composition, and this liquid is in the time of 55 ℃, and pressure is underpressure distillation under the 7KPa condition, behind volatilization water outlet and the ethanol, the 20g jelly, major ingredient is mixtures such as tannin, alkaloid, can adopt conventional extraction, smart/slightly the mode of heating up in a steamer is separated purification; The solids 460g that again solid-liquid separation is come out puts into reactor once more, and adding 60 ℃, concentration is the aqueous ethanolic solution 2L of 50 volume %, with microwave 2450MHz/1000W and ultrasonic wave 50KHz/500W, acting in conjunction, after handling 10min simultaneously, temperature reaches 180 ℃, and pressure reaches 2.0MPa, the decompression steam bleeding, filtering separation in the time of 90 ℃, the solid substance that solid-liquid separation is come out are the Semen Maydis cellulose pulp, after 120 ℃ of alcohol steam washings, surveying its polymerization degree is 700～900, and dry back is 242g; After the liquid that solid-liquid separation is come out is cooled to 50 ℃, generation xylogen precipitation, after filtering, whizzer gets xylogen 80g, surplus liquid is through atmospheric distillation tower, to get concentration be 35 volume % acetate, formic acid mixtures 0.02L to cut in the time of 120 ℃, and cut obtains concentration 50 volume % chaff aldehyde 0.2L in the time of 165 ℃.
Claims (3)
1. the separating process of an organic constituent of biomass is characterized in that, this method comprises the steps:
(1), be raw material with biomass, and pulverize, with the aqueous solutions of organic solvent infiltration of 20 volume %～70 volume % concentration, be that 900MHz～2500MHz, power are microwave treatment 5～30min of 700W～5000W with the frequency; The aqueous solutions of organic solvent that adds 20 volume %～70 volume % concentration again, make the biomass particle immerse in the aqueous solutions of organic solvent fully, at 40～120 ℃, pressure is under 0.4MPa～0.6Mpa condition, be 15KHz～2.4MHz with frequency again, power is that ultrasonic wave and the frequency of 200W～5000W is 900MHz～2500MHz, power is the microwave of 700W～5000W, handle 5～30min simultaneously, filtering separation then, wherein, biomass are unit with g, aqueous solutions of organic solvent is unit with L, and the volumetrical ratio of the weight of biomass starting material and above-mentioned twice total consumption of aqueous solutions of organic solvent is 500～1000: 0.8～3;
(2), the solid that filtering separation in the step (1) is obtained adds in the aqueous solutions of organic solvent of 20 volume %～70 volume % concentration, wherein, the solid that filtering separation obtains is unit with g, aqueous solutions of organic solvent is unit with L, and the solid weight that filtering separation obtains and the volumetrical ratio of aqueous solutions of organic solvent consumption are 500～1000: 0.8～3; At 160～220 ℃, pressure is under 1.2MPa～2.6MPa condition, with the frequency is that 15KHz～2.4MHz, power are the ultrasonic wave of 200W～5000W, frequency is that 900MHz～2500MHz, power are that the microwave of 900W～5000W is handled 5～30min simultaneously, carry out solid-liquid separation, the solids that obtains is a Mierocrystalline cellulose;
(3), the liquid after the solid-liquid separation, when cooling 60 ℃～normal temperature, produce the xylogen throw out, the xylogen throw out is through centrifugal treating, it is the xylogen finished product that its solids and pure water mix the solids that obtains after filtering again;
Wherein, described biomass are one or more in roots of plants, stem, the leaf part, and described aqueous solutions of organic solvent is any one in methanol aqueous solution, the aqueous ethanolic solution.
2. the separating process of organic constituent of biomass according to claim 1, it is characterized in that: in the described step (1), the liquid that filtering separation obtains carries out underpressure distillation at 40～80 ℃, air pressure under 2KPa～10KPa condition, evaporate fully until organic solvent, obtaining organism is the mixture that comprises tannin, pigment, alkaloid, essential oil, pectin.
3. the separating process of organic constituent of biomass according to claim 1 and 2, it is characterized in that: in the described step (3), the liquid that obtains through centrifugal treating, filtration treatment is sent in the distillation tower and is distilled, and collects acetate, furfural respectively, and resistates is oligose and wood sugar.
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