CN101274946A - Method for extracting lignose from crops leftovers - Google Patents
Method for extracting lignose from crops leftovers Download PDFInfo
- Publication number
- CN101274946A CN101274946A CNA2007100541587A CN200710054158A CN101274946A CN 101274946 A CN101274946 A CN 101274946A CN A2007100541587 A CNA2007100541587 A CN A2007100541587A CN 200710054158 A CN200710054158 A CN 200710054158A CN 101274946 A CN101274946 A CN 101274946A
- Authority
- CN
- China
- Prior art keywords
- extracting
- xylogen
- extraction
- filtrate
- micro
- Prior art date
- 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.)
- Pending
Links
Abstract
The invention provides a method for extracting lignin from the leftover bits and pieces of crops, which relates to the extraction field of effective components and is characterized in that the leftover bits and pieces of crops are ground, soaked in an extracting agent and then switched to a micro-wave extracting reactor for micro-wave radiant heating and extracting. The power of micro-wave radiant heating is 300W to 800W and the extracting time of micro-wave radiation is 30min to 40min. The extracting agent is high boiling point alcohol with a boiling point higher than 180 DEG C; the proportion between the added quantity of the extracting agent and materials is 10:1(volume weight ratio). The method provided by the invention can retain the original activity and the use value of the lignin and has the advantages of speediness, saving energy and high efficiency; the extracting agent can be recycled through distillation and nearly no pollutant is discharged.
Description
Technical field
The present invention relates to the extraction field of effective constituent in the crops leftovers, particularly a kind of microwave radiation of utilizing is extraction agent extracts xylogen from tankage such as agricultural crop straw, shell method with the high-boiling point alcohol.
Background technology
Xylogen is the natural high molecular substance with phenol type structure, its basic structural unit is the phenylpropyl alcohol alkyl, specifically, be the macromole that is formed by connecting with forms such as C-C key, C-O-C keys by pine and cypress alcohol radical, cloves base and three kinds of monomers of tonka-bean base with three-D space structure.
Contain phenolic hydroxyl group, alcoholic extract hydroxyl group, methoxyl group, aldehyde radical and carbonyl isoreactivity group in the lignin structure, modified-reactions such as oxidation, reduction, sulfomethylation, alkoxide, alkylation can take place under certain condition with some other compound, thereby are widely used in industry.Can prepare tackiness agent and synthetic resins with xylogen, as formaldehyde lignin resin, furfural lignin resin etc.In rubber industry, xylogen can be used as the weighting agent and the strengthening agent of rubber, replaces more expensive traditional strengthening agent carbon black, can reduce production costs.In petroleum industry, building materials industry, light industry all is widely used in the agricultural.
Xylogen extensively is present in xylophyta, herbaceous plant and the vascular plant, and content of lignin is 15%～25% in tankage such as the stalks of farm crop, shell.The tankage of these farm crop are generally as the material of biogas, feed of livestock or burning, abandon, and wherein xylogen is failed abundant extraction and application.And in the production of some medium and small papermaking enterprises, be paper making raw material with straw, rice straw, reed, bagasse mainly, xylogen becomes by product and is present in the papermaking wastewater, and at present to carry out the alkali recovery difficult very big for papermaking wastewater, xylogen is discharged with papermaking wastewater, has become environmental pollutant.
In plant materials, xylogen and Mierocrystalline cellulose and its hetero-organization link together.The method that lignin separation is come out has a lot, can be divided into two classes substantially.The first kind is that the dissolving of the composition beyond the xylogen in the plant materials is removed, and xylogen is filtered as insoluble composition and separates; Second class is then opposite, and xylogen is as soluble components, with lignin dissolution in the plant materials and other compositions such as Mierocrystalline cellulose do not dissolve the separation of carrying out.All there are some shortcomings in the concrete means of present two class separation methods.
Logical common acid (sulfuric acid or hydrochloric acid) is handled in first kind method.Mierocrystalline cellulose is hydrolyzed into glucose, and xylogen is separated as hydrolytic residue.Exemplary is exactly to use acid hydrolysis timber in the wood saccharification industry, and xylogen is subjected to the effect of acid in sepn process, and great changes will take place for its structure, lost certain activity and using value.When also not having good method to utilize xylogen, xylogen have to produce a large amount of acid waste liquids simultaneously as solid waste discharge, serious environment pollution.
Exemplary in second class methods is exactly the pulping process of papermaking.Main sulphite process (acid system) and the sulphate process (alkaline process) of adopting obtains water miscible sulfonated lignin and alkali lignin respectively in the paper industry, and Mierocrystalline cellulose is then separated out, and leaches Mierocrystalline cellulose, and remaining promptly is spent pulping liquor.Contain unserviceable xylogen in the spent pulping liquor, environment has seriously been polluted in the discharging of spent pulping liquor.
Also available organic solvent extraction in second class methods.Though these means can not produce waste liquid (organic solvent is recyclable), in extraction process the structural changes of xylogen also little, the extraction time is long, takes time and effort, and wastes energy, and does not meet the principle of saving the energy.
Therefore, but find the method for the extraction xylogen of easy, efficient, economical rationality suitability for industrialized production,, satisfy the market requirement of xylogen for making full use of tankage such as agricultural crop straw, shell, and administer the environmental pollution that causes in the medium and small papermaking enterprise production, have important value.
Summary of the invention
The present invention is intended to solve the problem that prior art exists, and provides a kind of extraction time short, energy-efficient, free of contamination, and utilizing microwave radiation is extraction agent extracts xylogen from crops leftovers method with the high-boiling point alcohol.
The invention discloses a kind of method of from crops leftovers, extracting xylogen, it is characterized in that, crops leftovers is pulverized, be soaked in the extraction agent, change over to then in the microwave extracting reactor, the carry out microwave radiation heating extraction.Get filtrate and filter residue after the reaction, filter residue washs through extraction agent, and washing lotion and filtrate merge, and the water that at room temperature adds 2～5 times of volumes also stirs in filtrate, promptly has the xylogen precipitation to separate out, centrifugation, and the collecting precipitation lyophilize promptly gets pulverous xylogen.
Difference according to tankage such as the stalks of used farm crop or shells, described carry out microwave radiation heating power is 300W～800W, the extraction time of microwave radiation is between 30min～40min, described extraction agent be boiling point at the high-boiling point alcohol more than 180 ℃, extraction agent add-on and material's proportion are 10: 1 (envelope-bulk to weight ratio).
Method provided by the invention utilizes microwave radiation to add extraction heat, has quick, energy-conservation, characteristics of high efficiency.The lignin structure that the present invention extracts does not have to change substantially, has the advantage that keeps original activity of xylogen and use value; The present invention is raw materials used to be tankage such as agricultural crop straw, shell, has utilization of waste material, the advantage that turns waste into wealth; The used extraction agent of the present invention is an organic solvent, can reclaim by distillation, and basic contamination-free is discharged, and has zero release, free of contamination advantage.Method provided by the invention replaces existing acid system or alkali paper-making pulping process as being used for medium and small paper mill, can reduce pollution greatly.
Embodiment
Embodiment 1, in the round-bottomed flask of 1000mL, add 50g through pulverizing the wheat straw stalk and 556mL 90% 1, the 4-butyleneglycol aqueous solution.Round-bottomed flask places the microwave extracting reactor, and the stream device is linked back outward.Carry out microwave radiation heating power is decided to be 640W, and the carry out microwave radiation heating time is 35min.After reaction finished, filter reaction mixture got filtrate and filter residue, filter residue with 80 ℃ 90% 1,4-butyleneglycol solution washing three times, the merging of washing lotion and filtrate.The water that at room temperature adds 3 times of volumes is in filtrate and stir about 20min, promptly has the xylogen precipitation to separate out.Centrifugation, collecting precipitation, lyophilize promptly gets the xylogen of brown ceramic powder shape.Filtrate is sloughed moisture under the underpressure distillation condition, be concentrated to contain butyleneglycol about 90%, recycles again.
Embodiment 2, in the round-bottomed flask of 1000mL, add 50g through the offal of pulverizing and the aqueous glycol solution of 556mL 90%.Round-bottomed flask places the microwave extracting reactor, and the stream device is linked back outward.Carry out microwave radiation heating power is decided to be 640W, and the carry out microwave radiation heating time is 30min.After reaction finished, filter reaction mixture got filtrate and filter residue, and filter residue washs three times with 80 ℃ 90% aqueous glycol solution, and washing lotion and filtrate merge.The water that at room temperature adds 3 times of volumes is in filtrate and stir about 20min, promptly has the xylogen precipitation to separate out.Centrifugation, collecting precipitation, lyophilize promptly gets the xylogen of brown ceramic powder shape.Filtrate is sloughed moisture under the underpressure distillation condition, be concentrated to contain ethylene glycol about 90%, recycles again.
Claims (3)
1. a method of extracting xylogen from crops leftovers is characterized in that, crops leftovers is pulverized, be soaked in the extraction agent, change over to then in the microwave extracting reactor, the carry out microwave radiation heating extraction gets filtrate and filter residue after the reaction, filter residue washs through extraction agent, washing lotion and filtrate merge, and the water that at room temperature adds 2～5 times of volumes also stirs in filtrate, promptly have the xylogen precipitation to separate out, centrifugation promptly gets pulverous xylogen.
2. in accordance with the method for claim 1, it is characterized in that described carry out microwave radiation heating power is 300W～800W, the extraction time is between 30min～40min.
3. in accordance with the method for claim 1, it is characterized in that, described extraction agent be boiling point at the high-boiling point alcohol more than 180 ℃, extraction agent add-on and material's proportion are 10: 1 (envelope-bulk to weight ratio).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100541587A CN101274946A (en) | 2007-03-29 | 2007-03-29 | Method for extracting lignose from crops leftovers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100541587A CN101274946A (en) | 2007-03-29 | 2007-03-29 | Method for extracting lignose from crops leftovers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101274946A true CN101274946A (en) | 2008-10-01 |
Family
ID=39994835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100541587A Pending CN101274946A (en) | 2007-03-29 | 2007-03-29 | Method for extracting lignose from crops leftovers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101274946A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219909A (en) * | 2011-04-25 | 2011-10-19 | 安徽农业大学 | Method for extracting lignin from pear pulp and purifying the lignin |
| CN101941993B (en) * | 2009-07-06 | 2013-08-21 | 中国科学院过程工程研究所 | Method for comprehensively utilizing cellulose and lignin of straws subjected to pentose extraction |
| US10240006B2 (en) | 2014-05-01 | 2019-03-26 | Renmatix, Inc. | Upgrading lignin from lignin-containing residues through reactive extraction |
| CN116376032A (en) * | 2022-12-30 | 2023-07-04 | 鲁东大学 | Biomass-based emulsifier for waterborne epoxy anticorrosive coating resin and preparation method thereof |
-
2007
- 2007-03-29 CN CNA2007100541587A patent/CN101274946A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941993B (en) * | 2009-07-06 | 2013-08-21 | 中国科学院过程工程研究所 | Method for comprehensively utilizing cellulose and lignin of straws subjected to pentose extraction |
| CN102219909A (en) * | 2011-04-25 | 2011-10-19 | 安徽农业大学 | Method for extracting lignin from pear pulp and purifying the lignin |
| US10240006B2 (en) | 2014-05-01 | 2019-03-26 | Renmatix, Inc. | Upgrading lignin from lignin-containing residues through reactive extraction |
| CN116376032A (en) * | 2022-12-30 | 2023-07-04 | 鲁东大学 | Biomass-based emulsifier for waterborne epoxy anticorrosive coating resin and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101864683B (en) | Pretreatment method of wood fiber raw materials | |
| CN102561082B (en) | Method of extracting hemicellulose, cellulose and lignin from wood fiber raw materials | |
| CN101285106B (en) | Process for preparing multicomponent liquid glucose and lignose while effectively hydrolyzing lignocellulosic biomass | |
| CN101580522B (en) | Method for separating lignin and cellulose from lignocellulose by using ionic liquid solvent | |
| CN101092435B (en) | Technical method for separating organic constituent of biomass | |
| CN102864672B (en) | Method for extracting lignin | |
| CN105504191A (en) | Preparation method of eutectic ionic liquid modified lignin-phenolic resin | |
| CN100348635C (en) | Shell biolobic material phenolic resin and its preparation method | |
| CN102101915B (en) | Separation method for agriculture and forestry biomass components | |
| CN102604121A (en) | Method for preparing high-quality lignin by coupling hydrothermal pretreatment and high-boiling-point alcohol | |
| CN101792495A (en) | Method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws | |
| CN102690423B (en) | Method for producing sodium lignosulphonate by utilizing residues obtained by producing ethanol with crop straws as raw materials | |
| CN106854264A (en) | A kind of rice husk sill quality modified phenolic resin adhesive preparation method | |
| CN105884907A (en) | Method for separating components of straws to prepare ultralow-viscosity carboxymethyl cellulose | |
| CN100500989C (en) | Full component separation for cell wall of agricultural refuse | |
| CN101274946A (en) | Method for extracting lignose from crops leftovers | |
| CN104164801A (en) | Method for separating and recycling cellulose, semicellulose and lignin in lignocellulosic biomass at one time | |
| CN106702802A (en) | Method for extracting high-purity cellulose from stalks in ionic liquid-sulfamic acid binary system | |
| CN103131017A (en) | Process for extracting lignin from lignocellulose biomass | |
| CN105906398A (en) | Method for preparing organic fertilizer through processing agriculture and forestry wastes by using organic solvent | |
| CN110041446B (en) | Comprehensive refining method for biomass | |
| WO2022052775A1 (en) | Production process of non-adhesive formaldehyde-free fiber board for straw co-production of fulvic acid | |
| CN114085252A (en) | Comprehensive utilization method for separating wood fiber by organic acid catalysis two-phase system | |
| CN106750360A (en) | A kind of method of the reverse solution system separating lignin of utilization alkali ionic liquid | |
| CN103194504B (en) | Application of sulfonated lignin in wood fibre material enzyme hydrolysis saccharification |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20081001 |