CN108221432A - A kind of process that cellulose is extracted from Suaeda salsa - Google Patents
A kind of process that cellulose is extracted from Suaeda salsa Download PDFInfo
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- CN108221432A CN108221432A CN201711455141.2A CN201711455141A CN108221432A CN 108221432 A CN108221432 A CN 108221432A CN 201711455141 A CN201711455141 A CN 201711455141A CN 108221432 A CN108221432 A CN 108221432A
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- cellulose
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- suaeda salsa
- filtrate
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- 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
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- 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
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- 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
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- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/003—Pulping cellulose-containing materials with organic compounds
Abstract
The present invention relates to cellulose extractive technique field more particularly to a kind of process that cellulose is extracted from Suaeda salsa, including hydrolysis pretreatment, ungrease treatment, individual composition, microwave treatment.The yield and purity of cellulose are improved using the process of the present invention.
Description
Technical field
The present invention relates to cellulose extractive technique field more particularly to a kind of techniques that cellulose is extracted from Suaeda salsa
Method.
Background technology
Alkali is fluffy also known as salt wormwood artemisia, seafood dish, is Chenopodiaceae annual herb salt tolerant euhalophyte, main fibre-bearing in cauline leaf
Element, aliphatic acid, leaf protein and Flavonoid substances.It is more to flavonoids Study on extraction in Suaeda salsa at present, from saline land alkali
The research of fluffy middle extraction cellulose is less, and the purity of cellulose is low, and yield is low, it is therefore necessary to establish a kind of from saline land alkali
The process of fluffy middle extraction cellulose.
Invention content
The technical problems to be solved by the invention are：In view of the deficienciess of the prior art, it provides a kind of from Suaeda salsa
The process of middle extraction cellulose, the cellulose purity using process extraction is high, and yield is high.
In order to solve the above technical problems, the technical scheme is that：
A kind of process that cellulose is extracted from Suaeda salsa, the described method comprises the following steps：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, adds in deionized water heating leaching
Bubble, the filter residue being collected by filtration pass through supercritical extract, using filtering, collect solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in extractant, by subcritical abstraction, centrifugation,
Solid-state filtrate is collected by filtration；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in organic acid soln and impregnates, through being overpressurized vapour
It steams, pH is adjusted to be stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after decatize, deionized water cleaning is taken, adds in acetic acid, Asia
Sodium chlorate and to pelargonyl group benzene sulfonic acid sodium salt, centrifuges after microwave treatment, filters, the filter residue of collection by it is dry be cellulose
Product.
As an improvement technical solution, the temperature of supercritical extract is 40-60 DEG C in step (1), time 30-
60min, extracting pressure 20-30Mpa.
As an improvement technical solution, in step (2) extractant be methanol, ethyl alcohol, n-butanol, ethyl acetate, benzene
At least one of.
As a kind of perferred technical scheme, mixed solution of the extractant for ethyl alcohol, ethyl acetate and benzene in step (2),
And the volume ratio of ethyl alcohol, ethyl acetate and benzene is 1-3.5:1:1-2.
As a kind of further improved technical solution, the volumetric concentration of the ethyl alcohol is 30%-60%.
As an improvement technical solution, for 40-65 DEG C, extraction time is the temperature of step (2) Subcritical extraction
30-60min, extracting pressure 0.5-2Mpa.
As an improvement technical solution, steam temperature is 105-140 DEG C in step (3), steaming time 0.5-
2.5h, the pressure of decatize is 0.15-0.25Mpa.
As an improvement technical solution, organic acid is acetic acid, citric acid or formic acid in step (3).
As an improvement technical solution, the temperature of microwave treatment is 70-110 DEG C, time 5-20s in step (4),
Power is 300-400w.
As an improvement technical solution, the filtrate tune pH to 4.2-4.8 that will be collected after step (4) centrifugal filtration adds
Enter the ethyl alcohol that volumetric concentration is 60%-80%, the precipitation that stirring, centrifugal filtration are collected is hemicellulose product by drying.
After employing above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Compared with prior art, the present invention mainly has the following advantages：
(1) present invention carries out the extraction of cellulose using Suaeda salsa as raw material, is pre-processed by hydrolyzing, utilizes overcritical extraction
Take technology that can effectively remove water-soluble component, leaf protein, water-soluble polysaccharide and some bioactive compositions；Pass through degreasing again
Processing, aliphatic acid, Flavonoid substances can be effectively removed using subcritical abstraction technology；Ethyl alcohol, ethyl acetate and benzene are as extraction
Agent, and according to 1-3.5:1:1-2 is mixed, and carries out degreasing to Suaeda salsa, degreasing effect is best；Again by decatize at
Reason, using vapor can be infiltered inside cell wall, and be condensed into liquid, released stress cold in rear cell wall at high temperature under high pressure
The evaporation suddenly of lime set body forms huge shearing force and then destroys the structure of cell wall so that the part hemicellulose in Suaeda salsa
Element degradation；It adds in acetic acid, sodium chlorite and to pelargonyl group benzene sulfonic acid sodium salt, by microwave-acid processing, can be promoted using microwave radiation
Intermolecular movement and friction, promote the degradation of hemicellulose molecule, while also destroy the change between macromolecular substances and polysaccharide
The combination of key is learned, therefore substantially increases the yield of cellulose, after the present invention is by hydrolyzing pretreatment and ungrease treatment, is carried significantly
The high purity of cellulose products.
(2) present invention handles the filtrate being collected by centrifugation after microwave-acid processing, can obtain hemicellulose product,
The purity of hemicellulose product may be up to 90.56%, and yield may be up to 0.282g/g Suaeda salsas.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Example 1
A kind of process that cellulose is extracted from Suaeda salsa, includes the following steps：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, add in the fluffy cauline leaf weight 5 of alkali
The deionized water heating of times volume is impregnated, the filter residue being collected by filtration by supercritical extract (temperature is 40 DEG C, time 30min,
Extracting pressure is 20Mpa), using filtering, collect solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in the extraction of solid-state filtrate 5 times of volumes of weight
(volumetric concentration is that the volume ratio of 30% ethyl alcohol, ethyl acetate and benzene is 1 for agent:1:1), by subcritical abstraction (temperature be 40 DEG C,
Extraction time is 30min, extracting pressure 0.5Mpa), it centrifuges, solid-state filtrate is collected by filtration；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in the organic of solid-state filtrate 8 times of volumes of weight
Sour (acetic acid) solution impregnates, and through being overpressurized decatize, (steam temperature is 107 DEG C, steaming time 0.5h, and the pressure of decatize is
0.15Mpa), pH is adjusted to be stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after decatize, deionized water cleaning is taken, adds in solid-state filtering
(volume ratio of acetic acid and sodium chlorite is 1 for the acetic acid of 8 times of volumes of object weight and the mixed liquor of sodium chlorite solution:1) it, adds
Solid-state filtrate weight 0.1% to pelargonyl group benzene sulfonic acid sodium salt, by microwave treatment, (temperature is 70 DEG C, time 5s, and power is
It 300w) centrifuges, filter afterwards, the filter residue of collection is by dry as cellulose products；
(5) the filtrate tune pH to 4.2 that will be collected after step (4) centrifugal filtration adds in the ethyl alcohol that volumetric concentration is 60%, stirs
It mixes, the precipitation that centrifugal filtration is collected passes through dry as hemicellulose product.
Under above-mentioned process conditions the yield of cellulose products be 0.24g/g Suaeda salsas, purity 88.4%,
The yield of hemicellulose product be 0.186g/g Suaeda salsas, purity 87.58%.
Example 2
A kind of process that cellulose is extracted from Suaeda salsa, includes the following steps：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, add in the fluffy cauline leaf weight 8 of alkali
The deionized water heating of times volume is impregnated, the filter residue being collected by filtration by supercritical extract (temperature is 48 DEG C, time 40min,
Extracting pressure is 22Mpa), using filtering, collect solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in the extraction of solid-state filtrate 8 times of volumes of weight
(volumetric concentration is that the volume ratio of 48% ethyl alcohol, ethyl acetate and benzene is 1.5 for agent:1:1.5), by subcritical abstraction, (temperature is
45 DEG C, extraction time 40min, extracting pressure 1Mpa), centrifuge, solid-state filtrate be collected by filtration；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in having for solid-state filtrate 10 times of volumes of weight
Machine acid (acetic acid) solution impregnates, and through being overpressurized decatize, (steam temperature is 120 DEG C, steaming time 1h, and the pressure of decatize is
0.2Mpa), pH is adjusted to be stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after decatize, deionized water cleaning is taken, adds in solid-state filtering
(volume ratio of acetic acid and sodium chlorite is 2 for the acetic acid of 10 times of volumes of object weight and the mixed liquor of sodium chlorite solution:1), then add
Enter solid-state filtrate weight 0.2% to pelargonyl group benzene sulfonic acid sodium salt, by microwave treatment, (temperature is 80 DEG C, time 10s, work(
Rate is 315w) it centrifuges, filter afterwards, the filter residue of collection is by dry as cellulose products；
(5) the filtrate tune pH to 4.3 that will be collected after step (4) centrifugal filtration adds in the ethyl alcohol that volumetric concentration is 68%, stirs
It mixes, the precipitation that centrifugal filtration is collected passes through dry as hemicellulose product.
Under above-mentioned process conditions the yield of cellulose products be 0.263g/g Suaeda salsas, purity 88.59%,
The yield of hemicellulose product be 0.197g/g Suaeda salsas, purity 87.98%.
Example 3
A kind of process that cellulose is extracted from Suaeda salsa, includes the following steps：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, add in the fluffy cauline leaf weight 12 of alkali
The deionized water heating of times volume is impregnated, the filter residue being collected by filtration by supercritical extract (temperature is 53 DEG C, time 45min,
Extracting pressure is 26Mpa), using filtering, collect solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in the extraction of solid-state filtrate 10 times of volumes of weight
Taking agent, (volumetric concentration is that the volume ratio of 53% ethyl alcohol, ethyl acetate and benzene is 2.5:1:2), by subcritical abstraction, (temperature is
62 DEG C, extraction time 50min, extracting pressure 1.8Mpa), centrifuge, solid-state filtrate be collected by filtration；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in having for solid-state filtrate 12 times of volumes of weight
Machine acid (citric acid) solution impregnates, and through being overpressurized decatize, (steam temperature is 132 DEG C, steaming time 2h, and the pressure of decatize is
0.23Mpa), pH is adjusted to be stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after decatize, deionized water cleaning is taken, adds in solid-state filtering
(volume ratio of acetic acid and sodium chlorite is 3 for the acetic acid of 12 times of volumes of object weight and the mixed liquor of sodium chlorite solution:1), then add
Enter to pelargonyl group benzene sulfonic acid sodium salt, centrifuge, filter afterwards by microwave treatment (temperature is 108 DEG C, time 18s, power 360w),
The filter residue of collection is by dry as cellulose products；
(5) the filtrate tune pH to 4.68 that will be collected after step (4) centrifugal filtration adds in the ethyl alcohol that volumetric concentration is 75%,
The precipitation that stirring, centrifugal filtration are collected is by dry as hemicellulose product.
Under above-mentioned process conditions the yield of cellulose products be 0.396g/g Suaeda salsas, purity 89.99%,
The yield of hemicellulose product be 0.282g/g Suaeda salsas, purity 90.56%.
Example 4
A kind of process that cellulose is extracted from Suaeda salsa, includes the following steps：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, add in the fluffy cauline leaf weight 12 of alkali
The deionized water heating of times volume is impregnated, the filter residue being collected by filtration by supercritical extract (temperature is 60 DEG C, time 60min,
Extracting pressure is 30Mpa), using filtering, collect solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in the extraction of solid-state filtrate 12 times of volumes of weight
Taking agent, (volumetric concentration is that the volume ratio of 60% ethyl alcohol, ethyl acetate and benzene is 3.5:1:2), by subcritical abstraction, (temperature is
65 DEG C, extraction time 60min, extracting pressure 2Mpa), centrifuge, solid-state filtrate be collected by filtration；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in having for solid-state filtrate 15 times of volumes of weight
Machine acid (citric acid) solution impregnates, and through being overpressurized decatize, (steam temperature is 140 DEG C, steaming time 2.5h, and the pressure of decatize is
0.25Mpa), pH is adjusted to be stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after decatize, deionized water cleaning is taken, adds in solid-state filtering
(volume ratio of acetic acid and sodium chlorite is 3.5 for the acetic acid of 15 times of volumes of object weight and the mixed liquor of sodium chlorite solution:1), then
It adds in pelargonyl group benzene sulfonic acid sodium salt, is centrifuged afterwards, mistake by microwave treatment (temperature is 110 DEG C, time 20s, power 400w)
Filter, the filter residue of collection is by dry as cellulose products；
(5) the filtrate tune pH to 4.8 that will be collected after step (4) centrifugal filtration adds in the ethyl alcohol that volumetric concentration is 80%, stirs
It mixes, the precipitation that centrifugal filtration is collected passes through dry as hemicellulose product.
Under above-mentioned process conditions the yield of cellulose products be 0.378g/g Suaeda salsas, purity 89.89%,
The yield of hemicellulose product be 0.267g/g Suaeda salsas, purity 90.27%.
In order to preferably prove that the preparation method using the present invention can improve cellulose products purity to extract cellulose
And recovery rate, the present invention have done 3 comparative examples simultaneously.
Comparative example 1
It is not both with implementing 3, step (1) hydrolysis pretreatment is that using supercritical extract, remaining condition is not identical, above-mentioned work
The yield of cellulose products is 0.382g/g Suaeda salsas under the conditions of skill, and purity 83.67%, the yield of hemicellulose product is
0.263g/g Suaeda salsas, the purity of hemicellulose is 83.56%.
Comparative example 2
It is not both with implementing 3, that using subcritical abstraction, remaining condition is not identical, and gained cellulose obtains in step (2)
Rate is 0.384g/g Suaeda salsas, and the purity of cellulose is 82.81%；The yield of hemicellulose is 0.258g/g, hemicellulose
Purity is 82.87%.
Comparative example 3
With implementing 3 not to be both that step (3) is without using steam treatment, without adding in pelargonyl group benzene sulfonic acid in step (4)
Sodium, also that by being ultrasonically treated, remaining condition is not identical, the yield of cellulose products is 0.352g/g salt under above-mentioned process conditions
Ground alkali is fluffy, purity 84.39%, and the yield of hemicellulose product is 0.235g/g Suaeda salsas, and the purity of hemicellulose is
84.52%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of process that cellulose is extracted from Suaeda salsa, it is characterised in that the process includes following step
Suddenly：
(1) hydrolysis pretreatment：The fluffy cauline leaf of alkali of fresh picking is taken, cleans, be homogenized after removal of impurities, deionized water heating is added in and impregnates,
The filter residue being collected by filtration passes through supercritical extract, using filtering, collects solid-state filtrate；
(2) ungrease treatment：The solid-state filtrate that step (1) is taken to collect adds in extractant, by subcritical abstraction, centrifugation, filtering
Collect solid-state filtrate；
(3) individual composition：The solid-state filtrate that step (2) is taken to collect adds in organic acid soln and impregnates, and through being overpressurized decatize, adjusts
PH is stirred, the solid-state filtrate being collected by filtration is cleaned again with deionized water to alkalinity；
(4) microwave treatment：Solid-state filtrate of the step (3) after individual composition is taken, adds in acetic acid, sodium chlorite and to nonanoyl
Base benzene sulfonic acid sodium salt is centrifuged after microwave treatment, is filtered, and the filter residue of collection is by dry as cellulose products.
2. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(1) temperature of supercritical extract is 40-60 DEG C, time 30-60min, extracting pressure 20-30Mpa in.
3. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(2) extractant is at least one of methanol, ethyl alcohol, n-butanol, ethyl acetate, benzene in.
4. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(2) organic solvent is the mixed solution of ethyl alcohol, ethyl acetate and benzene in, and the volume ratio of ethyl alcohol, ethyl acetate and benzene is 1-
3.5:1:1-2。
5. a kind of process that cellulose is extracted from Suaeda salsa according to claim 4, it is characterised in that：It is described
The volumetric concentration of ethyl alcohol is 30%-60%.
6. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(2) temperature of Subcritical extraction is 40-65 DEG C, extraction time 30-60min, extracting pressure 0.5-2Mpa.
7. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(3) steam temperature is 105-140 DEG C, steaming time 0.5-2.5h in, and the pressure of decatize is 0.15-0.25Mpa.
8. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(3) organic acid is acetic acid, citric acid or formic acid in.
9. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：Step
(4) temperature of microwave treatment is 70-110 DEG C, time 5-20s, power 300-400w in.
10. a kind of process that cellulose is extracted from Suaeda salsa according to claim 1, it is characterised in that：It will
The filtrate tune pH to 4.2-4.8 collected after step (4) centrifugal filtration adds in the ethyl alcohol that volumetric concentration is 60%-80%, stir,
The precipitation that centrifugal filtration is collected is by dry as hemicellulose product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113249995A (en) * | 2021-05-20 | 2021-08-13 | 青岛大学 | Clean and efficient separation method for biomass cellulose single fibers and lignin |
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| CN1445412A (en) * | 2003-04-23 | 2003-10-01 | 绵阳市晟邦科技有限责任公司 | Pulping method of non-wood fibers with no black liquor drained off as well as its boiler |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
| CN103030816A (en) * | 2012-12-25 | 2013-04-10 | 济南圣泉集团股份有限公司 | Technique for extracting lignin from biomass raw materials |
| CN103898780A (en) * | 2012-12-25 | 2014-07-02 | 中粮营养健康研究院有限公司 | Biomass treatment method |
| CN105568729A (en) * | 2015-12-22 | 2016-05-11 | 齐鲁工业大学 | Method for extracting celluloses, hemicelluloses and lignins from pennisetum hydridum |
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- 2017-12-28 CN CN201711455141.2A patent/CN108221432B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1445412A (en) * | 2003-04-23 | 2003-10-01 | 绵阳市晟邦科技有限责任公司 | Pulping method of non-wood fibers with no black liquor drained off as well as its boiler |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
| CN103030816A (en) * | 2012-12-25 | 2013-04-10 | 济南圣泉集团股份有限公司 | Technique for extracting lignin from biomass raw materials |
| CN103898780A (en) * | 2012-12-25 | 2014-07-02 | 中粮营养健康研究院有限公司 | Biomass treatment method |
| CN105568729A (en) * | 2015-12-22 | 2016-05-11 | 齐鲁工业大学 | Method for extracting celluloses, hemicelluloses and lignins from pennisetum hydridum |
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| CN113249995A (en) * | 2021-05-20 | 2021-08-13 | 青岛大学 | Clean and efficient separation method for biomass cellulose single fibers and lignin |
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