CN1796656A - Semi-cellulose low polymer produced from fibrous farm dreges and other reyenerable Chemical substance - Google Patents
Semi-cellulose low polymer produced from fibrous farm dreges and other reyenerable Chemical substance Download PDFInfo
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- CN1796656A CN1796656A CNA2004100954425A CN200410095442A CN1796656A CN 1796656 A CN1796656 A CN 1796656A CN A2004100954425 A CNA2004100954425 A CN A2004100954425A CN 200410095442 A CN200410095442 A CN 200410095442A CN 1796656 A CN1796656 A CN 1796656A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
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Abstract
A method for producing semicellulose low polymer and other regenerating chemical substance from fibrous agricultural residue applies organic solvent such as xylan polyose and / or oligose in straw and other lignin cellulose residue to carry out beat for producing paper pulp and other regenerating chemical substance. It is an environmental protection method of production and it can reduce or eliminate field-burning of straw for protecting environment.
Description
Technical field
The present invention relates to a kind ofly be used to handle lignocellulosic material therefrom to obtain the method for useful chemical substance.
Background technology
Cereal production is in the world producing the rubbish and the residue of enormous quantity.This is included in straw and the cereal dust that causes in results, storage and the transportation.Prepare for the plantation of carrying out next season to the field, straw is burnt in the field usually.But such behavior has caused the serious environmental pollution, and therefore this behavior is under an embargo in many countries.
Cereal industry is low income now.A kind of method of reversing this situation and avoiding open country to burn is that these rubbish and residue are converted into vendible product, and these products can increase the income of peasant and secondary industry.
China has recognized that the value of this method since a plurality of centuries.In China, spread all over the cereal planting area, straw is used for producing in numerous little pulp factories the paper pulp of paper grade (stock) always.Unfortunately, be used for being produced by straw the methods of beating of paper pulp at present, promptly soda processes when being used for realizing the small-scale of sodium recovery economically, has produced serious pollution.The water that sewage the produced pollution of discharging from these factories forces China to close minimum straw making beating soda ash factory of several thousand families at the end of the nineties.
Be suitable for producing and write with printing paper, be used for the oilpaper of laminated material and circuit board product, and the paper pulp that is applicable to the packing purposes can be known as the technology of organic solvent making beating (organosolv pulping) and by the millet straw preparation, this method has a plurality of remarkable advantages to the cereal agricultural by a kind of.It does not produce environmental problem in essence; It is than the less capital intensive of sulfate process (Kraft Process); It is ideally suited in the biological group of non-timber type (biomass) making beating that will contain the high-load inorganic material, and it can advantageously operated under little a lot of scale than traditional beating process.
Can be improved by the recovery maximization that makes useful by-product such as lignin, acetic acid, wood sugar and furfural with the economic viability of millet straw as the little organic solvent making beating factory of raw material.The income that increases from process byproducts means the small-scale of the favourable operation of energy and the factory of few capital investment.
Some polysaccharide and compound sugar such as arabogalactan, glucan, dextran and pectin have suitable value and purposes in numerous industry and food applications.Their majorities serve as thickener, suspending agent and rheology control agent.The limb of broad leaf tree and annual plant such as cereal, sugarcane and mestha is contained the hemicellulose that is rich in xylan of main amount, also has cellulose and lignin.In these raw material, hemicellulose can be up to 1/3rd of wooden biological group dry weight, and wherein xylan partly accounts for 3/4ths of total hemicellulose weight.Though these lignocellulosic materials contain xylan Quito sugar and compound sugar, these are as yet in industrial preparation, because verified, be difficult to isolate them from the cellulose of close association and lignin and do not make them be degraded to monose simultaneously.If can produce xylan with rational output from the biological group of lignocellulosic material such as fibroid agriculture residues, then xylan will have a considerable application industrial.
Summary of the invention
The present invention has instructed a kind of mill solution from organic solvent making beating operation to reclaim the method for xylan base compound sugar and polysaccharide and paper pulp and other useful products.Lignocellulosic material can be any suitable material, even comprises straw and other agriculture residues.
According to first aspect, the invention provides a kind of method of lignocellulosic material that be used to handle with acquisition xylan base compound sugar and/or polysaccharide and paper pulp, comprising:
-contain the organic solvent solution of organic solvent and water by in the continuous flow upstream boiling vessel, making the lignocellulosic material contact, make the making beating of lignocellulosic material experience organic solvent, thereby produce paper pulp and the solution that contains xylan base compound sugar and/or polysaccharide,
-from boiling vessel, remove the solution that comprises xylan base compound sugar and/or polysaccharide, and
-recovery xylan base compound sugar and/or polysaccharide from solution.
By under the continuous flow upstream pattern, carrying out this processing, just may control the condition (especially time) of lignocellulosic material and organic solvent solution period of contact modestly with adverse current boiling vessel such as screw feeding boiling vessel.The hemicellulose part of dissolving forms the back quilt at it and removes from the high-temperature area of organic solvent reactor rapidly.In case remove from reactor, when solution was flashed to environment temperature, the rapid reduction of temperature had suitably suppressed further hydrolysis.Environment temperature is meant the temperature that is lower than temperature in the boiling vessel.It may be a room temperature, perhaps is not easy to take place any other temperature of hydrolysis under this temperature when not having enzyme catalyst.Just can under the situation that further chemical conversion does not take place, carry out separation, purification and the recovery of various byproducts then.As its result, lignocellulosic material can be processed removing xylan base compound sugar and/or polysaccharide, and can not resolve into numbers of constituent monosaccharides.
Except in the adverse current boiling vessel, implementing this method (thereby can control the time of lignocellulosic material), further advantageously control the ratio of organic solvent in the organic solvent solution (as ethanol or other alcohol) and water with the organic solvent solution contact.By regulating the ratio of second alcohol and water, can make solution more positive or more not positive in hydrolysis.The bigger ethanol and the ratio of water will reduce the chemism of water, and will produce less hydrolysis, thereby make the polysaccharide in this technology keep the higher degree of polymerization.Therefore more hemicellulose will remain polysaccharide and compound sugar.Select the ratio of suitable second alcohol and water will produce the configuration of desirable polysaccharide, compound sugar and monose product in the mill solution.
Except the ratio degree of control organic solvent and water, can also control other factor, to obtain:
-xylan base compound sugar and/or polysaccharide, than
-monose and the product except xylan base compound sugar and/or polysaccharide
Desirable relative quantity.
These conditions are:
The ratio of organic solvent and water in-the organic solvent solution;
The time that-organic solvent solution and lignocellulosic material contact in the adverse current boiling vessel;
The pH value of-organic solvent solution; With
The temperature in-organic solvent making beating stage.
Preferably, they are controlled so that the recovery of xylan base compound sugar and/or polysaccharide maximizes, and these products are minimized to the hydrolysis or the conversion of monose such as wood sugar.Control these condition with the method for being instructed here, make the rate of recovery of xylan base compound sugar can reach at least 5%, and may be up to 7% or more with the initial dry weight basis of lignocellulosic material.The degree that wood sugar reclaims can be minimized to 4% or lower, and common about 2.5%.Arabinose and furfural content can reduce to respectively less than 0.5% and 1.0%.The output of mixing sugar (glucose and a spot of galactolipin) is very low usually, is generally about 2.2% with initial dry weight basis.
These aspects of the present invention are applied to any form of organic solvent beating method, and it generally comprises:
Under High Temperature High Pressure, biological group's fibrous material a period of time of boiling in the solution of the mixture that contains low molecular weight organic solvent and water, this time be enough at least in part biology be rolled into a ball fibrous material go wooden, and pulping,
From paper pulp, isolate the solution of using,
With the fresh solution washing pulp of organic solvent and water,
Reclaim the fresh solution of this second alcohol and water and use as solution circulated,
Processing is used for technology with the solution of crossing with recovery solvent and circulation and is also separated,
Purify and reclaim various chemical by-products, and
Reclaiming paper pulp handles in order to further standard.
This method can comprise the step of starch in the hydrolysis cereal dust, to be provided for producing the fermentable saccharide and other fermented product that can be used in this method of ethanol.
This method design is applicable to the lignocellulosic material that comprises sugarcane residue, millet straw residue, oil palm residue, and other lignocellulosic material that comprises any wooden biological group.The potential advantage of the present invention is to reclaim valuable renewable chemical substance, reduces the environmental hazard of organic solvent making beating operation, and can create the economically feasible little pulp factories of utilizing agriculture ligno-ccllulose residue.
Xylan is a kind of composition of hemicellulose, is a kind of polysaccharide.Xylan Quito sugar and/or compound sugar refer to any hydrolysis prods for the hemicellulose of compound sugar (comprising disaccharides) and/or polysaccharide derived from xylan, and it comprises xylan itself, does not comprise monose wood sugar and arabinose.
The organic solvent making beating of straw and other agriculture residues is incorporated in the independent making beating factory with the processing of multiple useful by-product and the fermentation of recovery and cereal processing-waste, will produces a large amount of incomes for cereal industry.Simultaneously such strategy will cause the environmental protection of high level and to the support based on the adjacent industrial activity development of the byproduct of this technology.This strategy has also been supported to change to the ideal of the New Times of regenerative resource and chemical substance from oil base, the fossil-carbon chemical substance of deriving.
The present invention is the compatibility of it and this industry to the other attraction of cereal industry.Its main technique chemical substance demand is a kind of organic solvent, and it may suitably be ethanol, and ethanol can be produced by the other products of process liquor such as the fermentation of the useless starch of hydrolysis simply.In addition, the many byproducts in this method for example have direct purposes and value in animal feed additive and slow release fertilizer and the pesticide in agricultural.
Description of drawings
Fig. 1 is the schematic flow sheet of a suitable embodiment of the inventive method.
The specific embodiment
Describe the present invention in detail with reference to Fig. 1, Fig. 1 is the schematic flow sheet of a suitable embodiment of the inventive method.
In organic solvent making beating operation, can be that the lignocellulosic material 1 of dry rice straw or other wooden biological group is transported to processing factory in the mode of routine, and be stored in an appropriate containers such as the feed bin 2.
In a preferred embodiment, dry rice straw is cut into short part, is transported in the continuous flow upstream tubular type boiling vessel 3.In a technology that is called pre-steaming, lignocellulosic material suitably is heated to a temperature that is lower than temperature in the boiling vessel.This pre-steaming should as far as possible promptly be operated, and preferably is less than 5 minutes.Extensively pre-avoiding and should avoiding of steaming, but pre-fast the steaming helps to remove the air that can cause disadvantageous oxidation reaction in boiling vessel from unprocessed lignocellulosic material.
In boiling vessel 3, under 175 ℃～185 ℃ (preferred 177 ℃～182 ℃), the lignocellulosic material 1 and the organic solvent solution (being the aqueous solution of ethanol in this case) of debita spissitudo (mixture of 35%～70%w/w suitably is 55～70%) were pulled an oar about 1～2 hour.From Fig. 1, can find, solution fresh, clean, heat shown in boiling vessel 3 right-hand side tops enter.Enter at boiling vessel left-hand side top via the forced feed device through the pre-lignocellulosic material that steams.This lignocellulosic material upwards is transported to the right side by the helix transporting device of inside from the left side, and organic solvent solution passes through boiling vessel downwards from right to left by the loose bed of ligno-ccllulose under gravity simultaneously.
After the boiling, the solution that part solution was promptly used is put to flash tank 4 from boiling vessel 3, also reclaimed the steam that is rich in ethanol, simultaneously paper pulp and some clean solution are put to blow-down tank 5 from boiling vessel in this condensation.
After blow-down tank 5 removes paper pulp, can make the coarse toilet paper slurry by a refiner or hydrabrusher, sieve and clean with conventional paper pulp process equipment (as washer 6), and as thick slurry (be collected in thick slurry jar 7 in), or be sent to according to and in the bleacher 8 that suitably designs as the required paper pulp type of final products.Here should be noted that than sulfate pulp ethanol based organic solvent paper pulp is easier to be bleached usually, so bleacher can have relatively simply design.In addition, organic solvent paper pulp has the output that is better than sulfate pulp usually.Dual disposal thing from bleaching stage can be handled with wet oxidation subsequently, to produce the sodium acetate of selling as commercial material.Because the integrated character of this method, such as the wet oxidation of other residue of the dust of handling derived from cereal can be in identical device simultaneously or carry out successively.
The ethanol water with crossing that will reclaim from boiling vessel concentrates in flash tank 4, and lignin settling tank 10 in and from acidifying stillage (will be further described below) mixing of destilling tower 9.The acetate that obtains from the latter half can be used for this acidifying.When the dilution of usefulness acidifying stillage, RICE STRAW LIGNIN is precipitated out from the solution with mistake, and can reclaim on drum-type filter 11.The lignin filter cake can be used on drum-type filter from the condensate shower of the cleaning of stillage evaporimeter and wash, and is dry in the drier 12 of suitably design then, packs 13 and sell afterwards.The form that this of lignin is pure has the purposes of multiple high value, comprises as the animal feed synergist, and as the natural in rubber, the grease.
Flow of solution from drum-type filter can add via tower feed pot 14 in the destilling tower 9, is used in technology recirculation to reclaim ethanol 15.Because normal process loss needs to replenish ethanol here.The bottomsstream (stillage) that can be by in evaporimeter 18, at first concentrating destilling tower (be collected in the stillage jar 16, and by decant 17) and provide required additional ethanol by inside.
Decant residual lignin in decanter 19, and in compound sugar recovery stage 20, remove xylan Quito sugar and compound sugar (this is a theme of the present invention) afterwards, by in conjunction with solvent extraction, solvent deposition and/or spatial exclusion chromatography, can replenish from processing factory and be rich in the effluent of nitrogen, phosphorus for residual solution.With waste gas carbohydrate or starch together, this solution can be used for the ethanol that technology is replenished to produce respectively, or produce mixed solvent (butanols/acetone) by yeast or anaerobe fermentation.Before this step, can from the stillage after concentrating, reclaim wood sugar.
Under the situation of alcohol production, the clear soup of fermentation can filter and and mix from the common ethanol that reclaims in the distillating material of lignin filter stream and the same tower.The stillage that reclaims since then is rich in acetic acid.When this stillage of evaporation, can reclaim unit 21 at the acetic acid that can partly be used for the lignin washing and reclaim the condensate that is rich in acetic acid, and being delivered to acetic acid, reclaims residue.Come the product of factory since then can partly be used for the stillage that acidifying is used for the lignin precipitation, and residue is sold, and perhaps mixes with wet oxidation solution, sells as sodium acetate as the acetic acid of food-grade.Market condition will determine the application of this material maximum value.The solid rich in proteins and the mineral matter that separate from the clear soup that ferments can be as a kind of suitable animal feed additives, or as the fertilizer of agriculture field.
Destilling tower is the recyclable ethanol that is used for recirculation not only, also recyclable furfural 22 and ethyl acetate, and this is two kinds of valuable products that produce during straw cooking.Their all may be sold as the thick product that is suitable for concentrating equipment to upgrade.Such activity will encourage to form additional local industry, and this industry is through designing to adopt method described in the present invention to support the cereal producer.Other local industry will be utilized the lignin of these plant produced, and convert it into value-added product, as concrete admixture and dye dispersant.
Other option comprises recovery wood sugar (a kind of many sugar that are present in a large number as xylan in the straw).In the world market selling owing to can be used for producing pure wood sugar, is the raw material that xylitol is produced as anti-dental caries sweetener.Wood sugar also can change into furfural.If the market price is supported this option, then wood sugar reclaims and maximizes and can realize by prolonging the boiling pre-steaming of straw before.Wood sugar will reclaim from pre-steaming condensate.
Utilize this option will produce the more paper pulp of high value,, therefore be applicable to the production of artificial fibre because they have high chemical cellulose content now.Result for cereal industry will eliminate expensive environment control measure, and produces the remarkable income from the sale of several value-added product.These products will be created the chance of introducing auxiliary industry conversely.
For the value and the flexibility of maximum, this method is operated in the adverse current boiling vessel, and has a further key element, promptly limits the ability of appropriate solvent and water ratio at the ideal product configuration.This organic solvent key element has produced such as lignin, wood sugar, furfural, acetic acid and has been used for the product of paper pulp, dietary fibre or the chemical cellulose of papermaking.Usually, when the ratio of ethanol and water is approximately 70%w/w, will produce higher levels of polysaccharide and compound sugar.Usually when 30～45% lower ethanol and water ratio, will produce more monose.
By the present invention, produced multiple value product in the solid residue by the cereal industry of adopting organic solvent making beating operation to be processed.In addition, the present invention will encourage to set up the new little organic solvent pulp factories of processing straw by strengthening the economic worth of these operations.The needs that this will reduce expensive straw residue treatment, reduced the convention of burning straw in essence---a kind ofly think environmentally harmful method of disposal at present.
Should be appreciated that, under the conditions without departing from the spirit and scope of the present invention, can carry out multiple change above-mentioned preferred implementation.
Claims (26)
1, a kind ofly be used to handle lignocellulosic material, comprise to obtain the method for xylan base compound sugar and/or polysaccharide and paper pulp:
-contain the organic solvent solution of organic solvent and water by in the continuous flow upstream boiling vessel, making the ligno-ccllulose contact, make the making beating of lignocellulosic material experience organic solvent, with production paper pulp and the solution that contains xylan base compound sugar and/or polysaccharide,
-from boiling vessel, remove the solution that contains xylan base compound sugar and/or polysaccharide, and
-recovery xylan base compound sugar and/or polysaccharide from solution.
2, according to the process of claim 1 wherein that the temperature of the solution of removing that contains xylan base compound sugar and/or polysaccharide is reduced to environment temperature fast from boiling vessel.
3,, control following condition so that xylan base compound sugar and/or polysaccharide minimize to the hydrolysis of wood sugar and other monose according to the process of claim 1 wherein:
The ratio of organic solvent and water in-the organic solvent solution;
The time that-organic solvent solution and lignocellulosic material contact in the adverse current boiling vessel;
The pH value of-organic solvent solution; With
The temperature in-organic solvent making beating stage.
4,, control following condition and be at least 5% the xylan base compound sugar rate of recovery to obtain initial dry weight basis with lignocellulosic material according to the process of claim 1 wherein:
The ratio of organic solvent and water in-the organic solvent solution;
The time that-organic solvent solution and hemicellulosic materials contact in the adverse current boiling vessel;
The pH value of-organic solvent solution; With
Temperature in the-organic solvent making beating stage.
5, according to the method for claim 4, wherein the xylan base compound sugar rate of recovery is at least 7 weight %.
6,, wherein control solvent contacts with ratio, organic solvent solution and the lignocellulosic material of water in the solution time, pH and temperature conditions, to obtain to be less than 4% the wood sugar rate of recovery according to the method for claim 4 or 5.
7, according to each method of claim 1～6, wherein the ratio of organic solvent and water is 30～70 weight % in the organic solvent solution.
8, according to the method for claim 7, wherein the ratio of organic solvent and water is 55～70 weight % in the organic solvent solution.
9, according to each method of claim 1～8, wherein organic solvent solution is 20～180 minutes with the time that lignocellulosic material contacts in boiling vessel.
10, according to the method for claim 9, wherein be 30～120 minutes contact time.
11, according to each method of claim 1～10, wherein the pH of organic solvent solution is 3.5～4.0.
12, according to each method of claim 1～11, wherein the temperature in organic solvent making beating stage is 170～205 ℃.
13, according to the method for claim 12, wherein this temperature is 177～182 ℃.
14, according to each method of claim 1～13, wherein the lignocellulosic material experience is pre-steams.
15,, wherein,, control the duration in pre-steaming stage according to xylan base compound sugar and/or polysaccharide desirable relative quantity with respect to monose and the product except xylan base compound sugar and/or polysaccharide according to the method for claim 14.
16, according to the method for claim 14 or 15, wherein pre-the steaming carried out 5 minutes or shorter, so that xylan base compound sugar and/or polysaccharide are reduced to minimum to the hydrolysis of wood sugar and other monose.
17, according to each method of claim 1～16, wherein this method comprises:
-reclaim xylan base compound sugar and/or polysaccharide by spatial exclusion chromatography and/or solvent precipitation.
18, according to each method of claim 1～17, wherein organic solvent is a primary alconol, or the mixture of alcohol.
19, according to each method of claim 1～18, wherein from the precipitation of the load flow of solution experience lignin of boiling vessel with separate, therefrom to reclaim lignin.
20, according to the method for claim 19, wherein after lignin recovery, flow of solution experience organic solvent is removed, and removing solvent from flow of solution, and recirculation is used for organic solvent solution.
21, according to the method for claim 20, wherein the removal of organic solvent is carried out in destilling tower.
22, according to the method for claim 21, wherein after organic solvent was removed, flow of solution experience acetic acid reclaimed.
23, according to the method for claim 22, wherein after acetic acid reclaimed, flow of solution experienced the recovery of xylan base compound sugar and/or polysaccharide.
24, according to the method for claim 23, wherein from flow of solution, reclaim the monose that comprises wood sugar.
25, according to each method of claim 22～24, wherein the acetic acid of Hui Shouing is used to precipitate lignin.
26,, wherein during organic solvent is removed, in destilling tower, reclaim furfural and/or ethyl acetate according to each method of claim 21～25.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2004100954425A CN1796656A (en) | 2004-12-22 | 2004-12-22 | Semi-cellulose low polymer produced from fibrous farm dreges and other reyenerable Chemical substance |
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| CNA2004100954425A CN1796656A (en) | 2004-12-22 | 2004-12-22 | Semi-cellulose low polymer produced from fibrous farm dreges and other reyenerable Chemical substance |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465373C (en) * | 2007-03-08 | 2009-03-04 | 上海交通大学 | Method of producing cellulose, lignin and xylose by biomass material |
| CN101725068A (en) * | 2008-10-29 | 2010-06-09 | 三星电子株式会社 | Method and device for fractionizing a biomass based on lignocellulose |
| WO2017107527A1 (en) * | 2015-12-25 | 2017-06-29 | 山东龙力生物科技股份有限公司 | Soluble dietary fiber and preparation method thereof |
| TWI717520B (en) * | 2017-05-26 | 2021-02-01 | 大陸商山東龍力生物科技股份有限公司 | Soluble dietary fiber and the producing method thereof |
-
2004
- 2004-12-22 CN CNA2004100954425A patent/CN1796656A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100465373C (en) * | 2007-03-08 | 2009-03-04 | 上海交通大学 | Method of producing cellulose, lignin and xylose by biomass material |
| CN101725068A (en) * | 2008-10-29 | 2010-06-09 | 三星电子株式会社 | Method and device for fractionizing a biomass based on lignocellulose |
| CN101725068B (en) * | 2008-10-29 | 2014-02-05 | 三星电子株式会社 | Method and device for fractionizing biomass based on lignocellulose |
| WO2017107527A1 (en) * | 2015-12-25 | 2017-06-29 | 山东龙力生物科技股份有限公司 | Soluble dietary fiber and preparation method thereof |
| CN106912964A (en) * | 2015-12-25 | 2017-07-04 | 山东龙力生物科技股份有限公司 | Soluble dietary fiber and preparation method thereof |
| KR20180081805A (en) * | 2015-12-25 | 2018-07-17 | 산동 롱라이브 바이오-테크놀로지 코., 엘티디 | Soluble fiber and process for making same |
| US10632136B2 (en) | 2015-12-25 | 2020-04-28 | Shandong Longlive Bio-Technology Co., Ltd | Soluble dietary fiber and preparation method thereof |
| KR102117175B1 (en) * | 2015-12-25 | 2020-05-29 | 산동 롱라이브 바이오-테크놀로지 코., 엘티디 | Soluble dietary fiber and method for its preparation |
| TWI717520B (en) * | 2017-05-26 | 2021-02-01 | 大陸商山東龍力生物科技股份有限公司 | Soluble dietary fiber and the producing method thereof |
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