CN106220755A - A kind of straw extracts reuse method - Google Patents
A kind of straw extracts reuse method Download PDFInfo
- Publication number
- CN106220755A CN106220755A CN201610663691.2A CN201610663691A CN106220755A CN 106220755 A CN106220755 A CN 106220755A CN 201610663691 A CN201610663691 A CN 201610663691A CN 106220755 A CN106220755 A CN 106220755A
- Authority
- CN
- China
- Prior art keywords
- straw
- steam explosion
- time
- separates
- seperator
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/14—Hemicellulose; Derivatives thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
- D21B1/021—Pretreatment of the raw materials by chemical or physical means by chemical means
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
- D21B1/30—Defibrating by other means
- D21B1/36—Explosive disintegration by sudden pressure reduction
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
The invention discloses a kind of straw and extract reuse method, relate to chemurgy technology field, the straw that harvesting is got off by (1) cuts into the length of 3 5cm, in the environment of 70 85 DEG C, adds organic solvent soaking 15min;(2) straw after soaking rinses 35 times, under the sun after dry in the sun 2 3h in water;(3) straw of preprocessed mistake is placed in steam explosion seperator, makes full use of straw, the most do not cause reagent waste simultaneously.
Description
Technical field
The present invention relates to chemurgy technology field, particularly relate to a kind of straw and extract reuse method.
Background technology
The crop growth cycle is short, yield big, and the straw as agricultural by product is an inexhaustible renewable sky of class
So resource.Biomass resource not only has recyclability, and has good biocompatibility and biodegradable.Mesh
Front straw is many is made ethanol etc. by whole utilization, such as straw power generation, crop straw burning, straw, and added value is low, only mends by state revenue and expenditure
Patch could maintain, hence in so that the utilization of straw is restricted.
Described straw, crops and Herba Medicaginis, the prairie milk vetch such as including Semen Tritici aestivi, Semen Maydis, Oryza sativa L., Cotton Gossypii, Sorghum vulgare Pers., Semen sojae atricolor, Semen arachidis hypogaeae
Deng water plants such as the stem after herbage harvesting reality, leaf, skin (shell) etc. and phragmites communiss.
General straw is mainly made up of cellulose, hemicellulose, lignin, and wherein content of cellulose is maximum, cellulose
Mass fraction is about 40%, and the mass fraction of lignin is about 25%, and the mass fraction of hemicellulose is about 20%;Straw also has
Mass fraction is about mineral and the protein etc. of 15%.Lead between cellulose, hemicellulose and lignin three component in straw
Cross the complicated chemistry such as chemical bond and hydrogen bond and non-bonding effect forms complicated supramolecular structure, it is difficult to separate and utilize;Half
Cellulose is easier to separate with other component in straw;And cellulose separates the technology difficulty being always in industry with lignin
Topic.
In recent years around Component seperation and the value added applications thereof of straw, carry out numerous studies work both at home and abroad.
The patent of invention of Publication No. " CN101463091A " discloses a kind of stalk carboxymethylation components and separates and prepare carboxymethyl fibre
The method of dimension element.In steam puffed stalk material, addition ethanol is as reaction medium, in the condition that sodium hydroxide and sodium chloroacetate exist
Under carry out carboxymethylation reaction, obtain containing carboxymethyl cellulose, carboxy methylation hemicellulose and the solid of carboxy methylation lignin.
By solid water-wet, add hydrochloric acid precipitation, add sodium hydroxide regulation pH, centrifugal collection supernatant and precipitation.Wash with ethanol
Washing supernatant and produce precipitation, carry out that sucking filtration obtains is precipitated as sodium carboxymethyl cellulose.Sediment fraction after Li Xin is carboxy methylation
Hemicellulose and lignin.This partly precipitated is carried out solvent extraction, be dissolved in solvent for carboxymethylated lignin, residue
For carboxymethylated hemicellulose.But at present these techniques yet suffer from environmental protection, component can not be completely separated, cost
Component high, that obtain is the problem such as carboxymethylation components rather than pure component (cellulose, hemicellulose, lignin).
The patent of invention that Authorization Notice No. is " CN101148830B " discloses one and straw is carried out steam explosion-microwave
The method of coupling processing separation straw component, step is as follows: after straw is carried out Steam explosion treatment, adds 40-60 DEG C of temperature
Water moistens washing of rising, and cleaning mixture staticly settles acquisition hemicellulose;Steam puffed stalk dehydration after washing is 3-5ml/ to water content
After g, then glycerol adding mixing, carry out intermittent microwave treatment;It is disposed, adds hot water insulated and stirred and dissolve 30-90min;Use 40-
60 DEG C of water wash filter 23-5 times, and filter cake is crude fibre;Filtrate is through staticly settling acquisition lignin.This separating technology is complicated, water
After washing, dehydration expends mass energy again;It addition, the method uses microwave treatment, microwave harm operator's is healthy.
The most relatively low to the utilization rate also ratio of straw, extract yield is low, production cost is high, environmental pollution is serious, therefore
Develop a kind of pollution-free, significant to the process that straw utilization rate is high..
Summary of the invention
For overcoming the deficiency in prior art, it is an object of the present invention to provide one and make full use of straw, do not cause simultaneously
The straw of reagent waste extracts reuse method.
For realizing the purpose of the present invention, technical scheme is as follows:
A kind of straw extracts reuse method, and described production method comprises the steps:
(1) straw that harvesting is got off is cut into the length of 3-5cm, in the environment of 70-85 DEG C, adds organic solvent soaking
15min, adds the sodium carboxymethyl cellulose of 0.1-2.0%, stirs;
(2) straw after soaking rinses 3-5 time, under the sun after dry in the sun 2-3h in water;
(3) being placed in steam explosion seperator by the straw of preprocessed mistake, adding mass fraction in described steam explosion seperator is
The alkali liquor of 0.5-10%, closes described seperator and is passed through steam, carries out steam explosion for the first time and separates;Described first time steam explosion separates
After, the material being blown off is carried out filter pressing, after filter pressing, gained the first clear liquid is the thick liquid of hemicellulose, collects first solid
Slag;
(4) being placed in steam explosion seperator by solid for gained first slag, adding mass fraction is the alkali liquor of 2-25%, closes steam explosion and separates
Machine is also passed through steam, the first solid slag is carried out second time steam explosion and separates;After described second time steam explosion separates, to be blown off
Material carries out filter pressing, and after filter pressing, gained the second clear liquid is the thick liquid of lignin, and after filter pressing, the solid slag of gained second is crude fibre.
Preferably, in described step (1), organic solvent is benzene/ethanol, normal hexane, chloroform or ether.
Preferably, in described step (3) and (4), alkali liquor is the aqueous solution of NaOH or KOH.
Preferably, in described step (3), temperature 20-200 DEG C of steam explosion separation for the first time, pressure 0.1-2MPa, time 5-
60min。
Preferably, in described step (4), temperature 80-260 DEG C of steam explosion separation for the second time, pressure 0.4-2.5MPa, time
5-200min。
Beneficial effects of the present invention: by straw Steam explosion treatment, first hemicellulose being separated, then remove
Residue outside hemicellulose expects Steam explosion treatment again, it is achieved cellulose and the separation of lignin.The method technique is simple, ring
Border is friendly, and low cost and hemicellulose, cellulose, lignin separation are thorough.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below in conjunction with
Detailed description of the invention, is expanded on further the present invention.
Embodiment 1:
A kind of straw extracts reuse method, and described production method comprises the steps:
(1) straw that harvesting is got off is cut into the length of 3cm, in the environment of 85 DEG C, adds organic solvent soaking 15min, add
The sodium carboxymethyl cellulose adding 0.1%, stirs;
(2) straw after soaking rinses 5 times, under the sun after dry in the sun 2h in water;
(3) being placed in steam explosion seperator by the straw of preprocessed mistake, adding mass fraction in described steam explosion seperator is 10%
Alkali liquor, close described seperator and be passed through steam, carrying out for the first time steam explosion and separate;After described first time steam explosion separates,
The material being blown off is carried out filter pressing, and after filter pressing, gained the first clear liquid is the thick liquid of hemicellulose, collects the first solid slag;
(4) being placed in steam explosion seperator by solid for gained first slag, adding mass fraction is the alkali liquor of 2%, closes steam explosion seperator also
It is passed through steam, the first solid slag is carried out second time steam explosion and separates;After described second time steam explosion separates, to the material being blown off
Carrying out filter pressing, after filter pressing, gained the second clear liquid is the thick liquid of lignin, and after filter pressing, the solid slag of gained second is crude fibre.
Organic solvent is benzene/ethanol, normal hexane, chloroform or ether;Alkali liquor is the aqueous solution of NaOH or KOH.
In step (3), the temperature 200 DEG C of steam explosion separation for the first time, pressure 0.1MPa, time 60min;In step (4), the
The temperature 260 DEG C of secondary steam explosion separation, pressure 0.4MPa, time 5min.
Embodiment 2:
A kind of straw extracts reuse method, and described production method comprises the steps:
(1) straw that harvesting is got off is cut into the length of 5cm, in the environment of 70 DEG C, adds organic solvent soaking 15min, add
The sodium carboxymethyl cellulose adding 2.0%, stirs;
(2) straw after soaking rinses 3 times, under the sun after dry in the sun 3h in water;
(3) being placed in steam explosion seperator by the straw of preprocessed mistake, adding mass fraction in described steam explosion seperator is
The alkali liquor of 0.5%, closes described seperator and is passed through steam, carries out steam explosion for the first time and separates;Described first time steam explosion separates complete
After, the material being blown off is carried out filter pressing, after filter pressing, gained the first clear liquid is the thick liquid of hemicellulose, collects the first solid slag;
(4) being placed in steam explosion seperator by solid for gained first slag, adding mass fraction is the alkali liquor of 25%, closes steam explosion seperator
And it is passed through steam, the first solid slag is carried out second time steam explosion and separates;After described second time steam explosion separates, to the thing being blown off
Material carries out filter pressing, and after filter pressing, gained the second clear liquid is the thick liquid of lignin, and after filter pressing, the solid slag of gained second is crude fibre.
Organic solvent is benzene/ethanol, normal hexane, chloroform or ether;Alkali liquor is the aqueous solution of NaOH or KOH.
In step (3), the temperature 20 DEG C of steam explosion separation for the first time, pressure 2MPa, time 5min;In step (4), for the second time
The temperature 80 DEG C of steam explosion separation, pressure 2.5MPa, time 200min.
Embodiment 3:
A kind of straw extracts reuse method, and described production method comprises the steps:
(1) straw that harvesting is got off is cut into the length of 4cm, in the environment of 78 DEG C, adds organic solvent soaking 15min, add
The sodium carboxymethyl cellulose adding 1%, stirs;
(2) straw after soaking rinses 4 times, under the sun after dry in the sun 2.5h in water;
(3) being placed in steam explosion seperator by the straw of preprocessed mistake, adding mass fraction in described steam explosion seperator is 5%
Alkali liquor, close described seperator and be passed through steam, carrying out for the first time steam explosion and separate;After described first time steam explosion separates,
The material being blown off is carried out filter pressing, and after filter pressing, gained the first clear liquid is the thick liquid of hemicellulose, collects the first solid slag;
(4) being placed in steam explosion seperator by solid for gained first slag, adding mass fraction is the alkali liquor of 16%, closes steam explosion seperator
And it is passed through steam, the first solid slag is carried out second time steam explosion and separates;After described second time steam explosion separates, to the thing being blown off
Material carries out filter pressing, and after filter pressing, gained the second clear liquid is the thick liquid of lignin, and after filter pressing, the solid slag of gained second is crude fibre.
Organic solvent is benzene/ethanol, normal hexane, chloroform or ether;Alkali liquor is the aqueous solution of NaOH or KOH.
In step (3), the temperature 100 DEG C of steam explosion separation for the first time, pressure 1MPa, time 30min;In step (4), second
The temperature 170 DEG C of secondary steam explosion separation, pressure 1.5MPa, time 100min.
Beneficial effects of the present invention: by straw Steam explosion treatment, first hemicellulose being separated, then remove
Residue outside hemicellulose expects Steam explosion treatment again, it is achieved cellulose and the separation of lignin.The method technique is simple, ring
Border is friendly, and low cost and hemicellulose, cellulose, lignin separation are thorough.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
Equivalent structure or equivalence flow process that bright description is made convert, or are directly or indirectly used in other relevant technology necks
Territory, is the most in like manner included in the scope of patent protection of the present invention.
Claims (5)
1. a straw extracts reuse method, it is characterised in that described production method comprises the steps:
(1) straw that harvesting is got off is cut into the length of 3-5cm, in the environment of 70-85 DEG C, adds organic solvent soaking
15min, adds the sodium carboxymethyl cellulose of 0.1-2.0%, stirs;
(2) straw after soaking rinses 3-5 time, under the sun after dry in the sun 2-3h in water;
(3) being placed in steam explosion seperator by the straw of preprocessed mistake, adding mass fraction in described steam explosion seperator is
The alkali liquor of 0.5-10%, closes described seperator and is passed through steam, carries out steam explosion for the first time and separates;Described first time steam explosion separates
After, the material being blown off is carried out filter pressing, after filter pressing, gained the first clear liquid is the thick liquid of hemicellulose, collects first solid
Slag;
(4) being placed in steam explosion seperator by solid for gained first slag, adding mass fraction is the alkali liquor of 2-25%, closes steam explosion and separates
Machine is also passed through steam, the first solid slag is carried out second time steam explosion and separates;After described second time steam explosion separates, to be blown off
Material carries out filter pressing, and after filter pressing, gained the second clear liquid is the thick liquid of lignin, and after filter pressing, the solid slag of gained second is crude fibre.
A kind of straw the most according to claim 1 extracts reuse method, it is characterised in that in described step (1), organic
Solvent is benzene/ethanol, normal hexane, chloroform or ether.
A kind of straw the most according to claim 1 extracts reuse method, it is characterised in that described step (3) and (4)
In, alkali liquor is the aqueous solution of NaOH or KOH.
A kind of straw the most according to claim 1 extracts reuse method, it is characterised in that in described step (3), and first
Temperature 20-200 DEG C of secondary steam explosion separation, pressure 0.1-2MPa, time 5-60min.
A kind of straw the most according to claim 1 extracts reuse method, it is characterised in that in described step (4), and second
Temperature 80-260 DEG C of secondary steam explosion separation, pressure 0.4-2.5MPa, time 5-200min.
Priority Applications (1)
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CN201610663691.2A CN106220755A (en) | 2016-08-15 | 2016-08-15 | A kind of straw extracts reuse method |
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CN201610663691.2A CN106220755A (en) | 2016-08-15 | 2016-08-15 | A kind of straw extracts reuse method |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108824050A (en) * | 2018-04-26 | 2018-11-16 | 东莞市泰昌纸业有限公司 | A kind of method that highly concentrated pulping reduces waste paper fibre damage in the process |
CN109338775A (en) * | 2018-09-30 | 2019-02-15 | 山东世纪阳光纸业集团有限公司 | A kind of closed loop environment-friendly stalk Biomechanical Pulping technique |
CN111672482A (en) * | 2020-06-30 | 2020-09-18 | 重庆工商大学 | Preparation method of carboxymethyl hemicellulose/chitosan cross-linked spherical hydrogel |
CN113331020A (en) * | 2021-07-16 | 2021-09-03 | 海南归耘田农业科技有限公司 | Method for treating rice straw |
-
2016
- 2016-08-15 CN CN201610663691.2A patent/CN106220755A/en not_active Withdrawn
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108824050A (en) * | 2018-04-26 | 2018-11-16 | 东莞市泰昌纸业有限公司 | A kind of method that highly concentrated pulping reduces waste paper fibre damage in the process |
CN108824050B (en) * | 2018-04-26 | 2020-08-18 | 东莞市泰昌纸业有限公司 | Method for reducing damage of waste paper fibers in high-concentration pulping process |
CN109338775A (en) * | 2018-09-30 | 2019-02-15 | 山东世纪阳光纸业集团有限公司 | A kind of closed loop environment-friendly stalk Biomechanical Pulping technique |
CN109338775B (en) * | 2018-09-30 | 2020-12-01 | 山东世纪阳光纸业集团有限公司 | Environment-friendly straw bio-mechanical pulping process |
CN111672482A (en) * | 2020-06-30 | 2020-09-18 | 重庆工商大学 | Preparation method of carboxymethyl hemicellulose/chitosan cross-linked spherical hydrogel |
CN113331020A (en) * | 2021-07-16 | 2021-09-03 | 海南归耘田农业科技有限公司 | Method for treating rice straw |
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Application publication date: 20161214 |