CN101811692B - New method for comprehensive utilization of straw resource - Google Patents
New method for comprehensive utilization of straw resource Download PDFInfo
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- CN101811692B CN101811692B CN201010162163A CN201010162163A CN101811692B CN 101811692 B CN101811692 B CN 101811692B CN 201010162163 A CN201010162163 A CN 201010162163A CN 201010162163 A CN201010162163 A CN 201010162163A CN 101811692 B CN101811692 B CN 101811692B
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Abstract
The invention discloses a new method for comprehensive utilization of straws, and in particular relates to a new method for separation of sugar acid solution in straw hydrolysis liquid and comprehensive utilization of a straw resource. When the problem of the separation of sugar acid is solved, a series of high value-added products such as biomass-based colloidal carbon spheres, nano carbon black, high specific area nano porous carbon spheres and high-energy organic carbon are prepared. The method comprises the following steps: hydrolyzing the straws by using organic acid at certain concentration, and filtering the mixture to obtain the sugar acid solution and filter residue; adjusting the concentration of the sugar acid solution, and performing polycondensation and carbonization reaction to prepare the colloidal carbon spheres; and thermally treating the prepared colloidal carbon spheres to form the nano carbon black; or activating the colloidal carbon spheres under certain conditions to form nano porous carbon with high specific area and strong adsorption capability. Compared with the colloidal carbon prepared from high molecular materials and cyclic polysaccharide, the biomass-based colloidal carbon spheres and other products prepared by the method have the characteristics of large raw material amount, reproduction, energy conservation, recycle of sulfuric acid and phosphoric acid, environmental protection of the whole process and the like.
Description
Technical field
The present invention relates to a kind of novel method of stalk resource comprehensive utilization, be specifically related to the novel method of a kind of biomass-based colloidal carbon sphere, nanometer porous carbon, nano carbon black, the preparation of high-energy organic carbon.
Background technology
Biomass are important renewable resources, and clean environmental protection, and China's biomass resource appearance volume is big, how to make full use of biomass resource, and it is turned waste into wealth becomes the focus of various countries' researcher research.At present, cause various countries' extensive concern around biomass by hydrolyzation comprehensive utilization aspect, main method for hydrolysis has two kinds: acid as catalyst dilute acid hydrolysis and concentrated acid hydrolysis, but all there is certain problem in these two kinds of hydrolysis.Problem one: the dilute acid hydrolysis condition needs HTHP, and plant factor and anticorrosion problem can't solve in industry; Problem two: concentrated acid hydrolysising condition low-temperature atmosphere-pressure, percent hydrolysis is high, helps industrial production, but has the isolating problem of saccharic acid in the hydrolyzed solution, and the problems referred to above become the bottleneck of restriction biomass as resources comprehensive utilization.The present invention adopts the chemosetting technology of biomass energy, resource to solve the saccharic acid separation problem, has realized the low-cost imagination that can make sour recycle.Carry out the serial application research of cured product simultaneously, for the comprehensive utilization biomass resource has been started a new method.The spherical carbon material is the lithium ion battery negative material of one type of very advantageous and potentiality in addition, and its research and development come into one's own day by day, utilizes biomass resource to prepare nanometer charcoal ball and will have important exploitation value.
Stalk is a kind of important biomass resource, and its kind volume is big.The annual product in whole world agricultural crop straw is more than 2,900,000,000 ton at present, and China can produce stalk every year and reach more than 700,000,000 tons.Wherein be example with the rice husk, annual about 200,000,000 tons of the paddy that produces of China is equivalent to 40,000,000 tons on rice husk, accounts for more than 30% of Gross World Product, ranks first in the world, and will bring bigger economic benefit and social benefit to us if made full use of these resources.But stalk resource is not fully utilized at present, and major part slatterns or directly burns as agricultural waste, causes environmental pollution.The present invention promptly is a series of high added value materials of feedstock production with the stalk.Chinese patent CN101020344A discloses a kind of working method and specific equipment thereof of straw biological honeycomb briquette; Its technical scheme is; With corn, soybean, wheat, cotton, rice straw, Pericarppium arachidis hypogaeae or sawdust, weeds, trees deadwood etc. is raw material; Become straw biological carbon through carbonizing treatment, mix with quartz sand, clay powder and water again, be pressed into honeycomb briquette.Chinese patent CN101139400A discloses the method that a kind of straw acetylized component separates and prepare cellulose acetate, and particular content is: in gas explosion stalk material, add isopyknic Glacial acetic acid min. 99.5 and diacetyl oxide; Under the sulfuric acid existence condition, carry out acetylize and handle, generation contains FM, acetylated hemicellulose and acetylize lignin liquid; This liquid is inserted in the whizzer centrifugal, supernatant and deposition, abandon deposition, stay supernatant; Add the water washing supernatant then and produce deposition, carrying out suction filtration again must precipitate, and water washing and precipitating is to neutral, and poach is dried then, must contain acetylize products such as FM, acetylize xylogen and acetylated hemicellulose; Acetylizad semicellulose and xylogen are used solvent extraction, and what be dissolved in solvent is Cellulose diacetate, acetylated hemicellulose and xylogen, and remaining is cellulosetri-acetate.Chinese patent CN101041834A discloses a kind of complete processing with straw, corn or broomcorn straw industrial production of ethyl alcohol.Concrete steps comprise with the rice straw machine be pressed into brick, through 0.5～2.0 * 10
6Gy's
60Co-gamma-rays or electron-beam accelerator radiotreatment, mechanical disintegration cross that 200 mesh sieves, hot water lixiviate, ethanol delignification, enzyme liberating separate with 1～2 micron nucleopore membranes, yeast saccharomyces cerevisiae and pichia spp synchronous saccharification disperse operations such as fermentation, ethanol dehydration separate.It is the method that raw material application enzyme and membrane technique prepare high-purity oligoxylose with the stalk that Chinese patent CN101003823A discloses a kind of; Concrete steps are: be raw material with the stalk, steam explosion handle the explosion stalk, add xylanase hydrolysis and handle; Centrifugal or mistake filters supernatant; Nanofiltration or vacuum concentration, s.t., centrifugal or mistake filters supernatant; Charcoal absorption, ultrafiltration and ion exchange resin treatment, concentrated or spraying drying prepares high-purity oligoxylose syrup or the Icing Sugar of xylooligosaccharides content 70%-90%.Above patent exists product single aspect straw utilization, complex process, and product is difficult for problems such as purifying.
The present invention adopts earlier stalk to be carried out s.t. on the basis of our previous work, utilizes its hydrolyzed solution to prepare the high added value material again, and the method for this kind straw utilization is not also seen patent report.
Summary of the invention
The object of the invention provides a kind of method of utilizing the stalk acid hydrolysis liquid to prepare a series of high value added products.
The present invention at first mixes stalk with 36～72% mineral acid by a certain percentage, is under 50～80 ℃ of conditions in temperature, and hydrolysis 10～40 minutes is crossed and filtered sugar acid solution and filter residue; The acid concentration of adjustment sugar acid solution is 10%～74%, is under 50～95 ℃ in temperature, polycondensation and carbonization reaction 0.5～6 hour; Or 120～200 ℃ of hydro-thermals in the reaction kettle, reacted 2～10 hours, filter; Solids wash, drying, colloidal carbon sphere or the colloid charcoal ball of preparation 200～1500nm; With colloidal carbon sphere for preparing in the above experiment and activator mix (mass ratio is 1: 1～6), oxygen barrier is warming up to 300～600 ℃, and washing, filtration, drying are taken out in activation 0.5～2 hour, preparation specific surface area 1700～3300m
2The nanometer porous carbon of/g has stronger adsorptive power.
Embodiment
Embodiment 1: with rice husk and 72%H
2SO
4By solid-to-liquid ratio is that 1: 10 (g/ml) mixes, and places 50 ℃ of water-bath hydrolysis 10 minutes, and regulating acid concentration is 42%, filters to obtain sugar acid solution; Again sugar acid solution is placed 60 ℃ of water-bath polycondensations 2 hours, 95 ℃ of water-bath carbonization reaction 6 hours, filtration, washing, drying are prepared the colloidal carbon sphere that particle diameter is 427nm.
Embodiment 2: the acid concentration that changes polycondensation and carbonization is 52%, other condition such as embodiment 1.Make the colloidal carbon sphere that particle diameter is 534nm.
Embodiment 3: hydrolysising condition is with embodiment 1, and the acid concentration of regulating sugar acid solution is 35%, places reaction kettle, and 160 ℃ of hydro-thermal reactions 6 hours, filtration, washing, drying were prepared the colloidal carbon sphere that particle diameter is 758nm.
Embodiment 4: hydrolysising condition is with embodiment 1, and the acid concentration of regulating sugar acid solution is 45%, places reaction kettle, and 160 ℃ of hydro-thermal reactions 6 hours, filtration, washing, drying were prepared the colloidal carbon sphere that particle diameter is 967nm.
Embodiment 5: the colloidal carbon sphere oxygen barrier of preparation among the embodiment 1 is warming up to 400 ℃, and constant temperature thermal treatment 1 hour obtains the nano carbon black that particle diameter is 425nm.
Embodiment 6: the colloidal carbon sphere oxygen barrier of preparation among the embodiment 3 is warming up to 500 ℃, and constant temperature thermal treatment 1 hour obtains the nano carbon black that particle diameter is 754nm.
Embodiment 7: hydrolysising condition is with embodiment 1, and the acid concentration of regulating sugar acid solution is 52%, places 95 ℃ of water-bath carbonization reaction 6 hours, filtration, washing, dryly must consolidate the charcoal product, and its combustion heat value is 24.5929MJ/Kg.
Embodiment 8: hydrolysising condition is with embodiment 1, and the acid concentration of regulating sugar acid solution is 62%, places 95 ℃ of water-bath carbonization reaction 4 hours, filtration, washing, dryly must consolidate the charcoal product, and its combustion heat value is 25.0574MJ/Kg.
Embodiment 9: hydrolysising condition is with embodiment 1, and the acid concentration of sugar acid solution is 72%, places 95 ℃ of water-bath carbonization reaction 2 hours, filtration, washing, dryly must consolidate the charcoal product, and its combustion heat value is 25.8239MJ/Kg.
Embodiment 10: the preparation condition of colloidal carbon sphere is with embodiment 1, with the colloidal carbon sphere and the H of preparation
3PO
4By mass ratio is mixing in 1: 2.5, and oxygen barrier is warming up to 500 ℃, constant temperature priming reaction 1 hour, and it is 2700m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 1.3cm
3The activated carbon product of/g.
Embodiment 11: the preparation condition of colloidal carbon sphere is with embodiment 1, with the colloidal carbon sphere and the H of preparation
3PO
4By mass ratio is mixing in 1: 2, and oxygen barrier is warming up to 500 ℃, constant temperature priming reaction 1.5 hours, and it is 2250m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 1.6cm
3The activated carbon product of/g.
Embodiment 12: the preparation condition of colloidal carbon sphere is with embodiment 1, with the colloidal carbon sphere and the H of preparation
3PO
4By mass ratio is mixing in 1: 4, and oxygen barrier is warming up to 500 ℃, constant temperature priming reaction 1 hour, and it is 2500m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 2.0cm
3The activated carbon product of/g.
Embodiment 13: the preparation condition of colloidal carbon sphere is with embodiment 1, with the colloidal carbon sphere and the H of preparation
3PO
4By mass ratio is mixing in 1: 2, and oxygen barrier is warming up to 450 ℃, constant temperature priming reaction 1 hour, and it is 2400m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 1.2cm
3The activated carbon product of/g.
Embodiment 14: the preparation condition of colloidal carbon sphere is with embodiment 1, with the colloidal carbon sphere and the H of preparation
3PO
4By mass ratio is mixing in 1: 4, and oxygen barrier is warming up to 550 ℃, constant temperature priming reaction 1 hour, and it is 2300m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 2.1cm
3The activated carbon product of/g.
Embodiment 15: the preparation condition of colloidal carbon sphere is with embodiment 1; Is to mix at 1: 4 colloidal carbon sphere and the KOH of preparation by mass ratio, and oxygen barrier is warming up to 400 ℃, constant temperature 0.5 hour; Be warming up to 800 ℃ of priming reactions again 1 hour, it is 2850m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 1.6cm
3The activated carbon product of/g.
Embodiment 16: the preparation condition of colloidal carbon sphere is with embodiment 1; Is to mix at 1: 3 colloidal carbon sphere and the NaOH of preparation by mass ratio, and oxygen barrier is warming up to 400 ℃, constant temperature 0.5 hour; Be warming up to 800 ℃ of priming reactions again 1 hour, it is 2350m that washing, filtration, drying obtain specific surface area
2/ g, pore volume are 1.5cm
3The activated carbon product of/g.
Claims (5)
1. stalk resource comprehensive utilization method, its concrete steps are following:
(1) at first with the mineral acid of stalk with 36～72wt%, be under 50～80 ℃ of conditions in temperature, hydrolysis 10～40 minutes is crossed and is filtered sugar acid solution and filter residue; The acid concentration of adjustment sugar acid solution is 10～72wt%, is under 50～95 ℃ in temperature, polycondensation and carbonization reaction 0.5～6 hour; Or in 120～200 ℃ of reaction kettles hydro-thermal reaction 2～10 hours; Filter solids wash, drying, the colloidal carbon sphere of preparation 200～1500nm;
(2) with the colloidal carbon sphere and the activator mix of preparation in (1), mass ratio is 1: 1～6, and oxygen barrier is warming up to 300～800 ℃, and washing, filtration, drying are taken out in activation 0.5～2 hour, and preparing specific surface area is 1700～3300m
2The nanometer porous carbon of/g.
2. stalk resource comprehensive utilization method as claimed in claim 1, it is characterized in that: acvator is phosphoric acid, Pottasium Hydroxide, sodium hydroxide.
3. stalk resource comprehensive utilization method as claimed in claim 1, it is characterized in that: described mineral acid is phosphoric acid, sulfuric acid or its mixed acid solution.
4. a stalk resource comprehensive utilization method as claimed in claim 1 is characterized in that: after the sugar acid solution polycondensation and carbonization, filter gained filtrating in the step (1), recycle after the adjustment acid concentration; With behind the phosphoric acid activation, the washing filtering gained is filtrated in the step (2), recycle after the adjustment acid concentration.
5. a stalk resource comprehensive utilization method as claimed in claim 1 is characterized in that: after the sugar acid solution polycondensation and carbonization, filter the gained filter residue in the step (1), according to the different preparation of raw material Different products; With rice husk, straw is raw material, and filter residue is through calcining preparation nano silicon; With the corn stalk is raw material, the activated preparation top-grade active carbon of filter residue.
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| CN201010162163A CN101811692B (en) | 2010-05-05 | 2010-05-05 | New method for comprehensive utilization of straw resource |
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