CN108951254A - A kind of method that bamboo hemicellulose efficiently separates - Google Patents
A kind of method that bamboo hemicellulose efficiently separates Download PDFInfo
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- CN108951254A CN108951254A CN201810742645.0A CN201810742645A CN108951254A CN 108951254 A CN108951254 A CN 108951254A CN 201810742645 A CN201810742645 A CN 201810742645A CN 108951254 A CN108951254 A CN 108951254A
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- hemicellulose
- bamboo
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- efficiently separates
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27J—MECHANICAL WORKING OF CANE, CORK, OR SIMILAR MATERIALS
- B27J1/00—Mechanical working of cane or the like
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K9/00—Chemical or physical treatment of reed, straw, or similar material
- B27K9/002—Cane, bamboo
-
- 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
- D21C1/00—Pretreatment of the finely-divided materials before digesting
- D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam
Abstract
The invention discloses a kind of methods that bamboo hemicellulose efficiently separates, comprising the following steps: (1) spare after over dry by bamboo wood cutting at small bamboo chip；(2) the small bamboo chip after weighing over dry is put into reactor, distilled water is added, and be heated to 145-170 DEG C, is then kept the temperature 0.5-2h, obtain extract；The pH to 3-5 for adjusting extract again continues to stop reaction after keeping the temperature 0.5-2h；(3) after liquid to be extracted is cooled to room temperature, filtrate is collected in filtering；(4) clear liquid is collected after centrifugation in filtrate, then be added ethanol solution repeat extraction 3 times to get.The present invention extracts hemicellulose using the hot water of preconditioning pH, promotes to inhibit the dissolution and degradation of cellulose and lignin while hemicellulose dissolution during the extraction process, to obtain the hemicellulose of high molecular weight, high yield pulp1.Separation method through the invention, hemicellulose yield are 38.44-46.00%, and wherein the hemicellulose of 63.18-93.39% exists in the form of glycan.
Description
Technical field
The present invention relates to biorefinery technical field more particularly to a kind of methods that bamboo hemicellulose efficiently separates.
Background technique
There are four elements for Wooden Biomass: extract, hemicellulose, lignin and cellulose.Each component
The ability of chemically-resistant, heat or biological degradability is not quite similar, and wherein hemicellulose degradation is easiest to, and cellulose is most difficult to degrade.
The difference that heterogeneity in biological respinse causes Wooden Biomass to be converted, therefore an optimum process is selected, to realize wooden life
Substance main component efficiently separate and conversion is necessary.Especially efficiently separating with higher value application especially with hemicellulose
Urgently.
Domestic correlative study has at present: Chinese patent 200980142580.5 discloses giantreed hemicellulose recycling side
Method, this method include that giantreed fragment is handled in the liquid at the temperature of 40~90 DEG C of ranges and 5~12 pH using it, are extracted
At most total available hemicellulose of one third, hemicellulose yield are lower；Chinese patent 201310042450.2 discloses half
Cellulose and preparation method thereof, this method are first to handle lignocellulosic material high-temperature sterilization, then access whiterot fungi and quiet
The culture different time period is set, then water-soluble hemicellulose is obtained with flooding to the biomass components after degradation, it is complicated for operation,
Hemicellulose yield is lower；Chinese patent 201210047241.2 discloses a kind of extraction separation method of hemicellulose, the party
Method pre-processes raw material using aqueous slkali, is decolourized, after extraction of flocculating, and obtained hemicellulose product is filtered in centrifugation, and product is pure
Change process is more complicated.
Summary of the invention
It is an object of the invention to: in view of the above problems, provide a kind of high molecular weight, the bamboo half fiber of high yield pulp1
The method that dimension element efficiently separates.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of method that bamboo hemicellulose efficiently separates, comprising the following steps:
(1) by bamboo wood cutting at small bamboo chip, placement is dried to over dry at 105 DEG C in an oven, then collects spare；
(2) the small bamboo chip after weighing over dry is put into reactor, distilled water is added, and be heated to 145-170 DEG C, is then protected
Warm 0.5-2h, obtains extract；The pH to 3-5 for adjusting extract again continues to stop reaction after keeping the temperature 0.5-2h；
(3) after liquid to be extracted is cooled to room temperature, filtrate is collected in filtering；
(4) clear liquid is collected after centrifugation in filtrate, ethanol solution is then added, sufficiently miscible rear stratification is collected
Upper layer of extraction liquid repeats extraction 3 times, is freeze-dried after extract liquor rotary evaporation in the environment of -60 DEG C to get the hemicellulose
Element.
Preferably, in step (1), the small a length of 20-40mm of bamboo chip, width 3-5mm.
Preferably, the weight ratio of small bamboo chip and distilled water after the over dry is 1:4-7 in step (2).
Preferably, the time of the heating is 0.5-1.5h in step (2).
Preferably, adjusting the pH of the extract using acetate buffer solution in step (2).
Preferably, the revolving speed of the centrifugation is 4500-5200rpm, and is centrifuged 8-12min under normal pressure in step (4).
Preferably, the ethanol solution is 2.5-3.5 times of the supernatant volume, the anhydrous second in step (4)
The mass fraction of alcohol is 95%.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
The method that bamboo hemicellulose of the invention efficiently separates extracts hemicellulose using the hot water of preconditioning pH, is mentioning
Promote dissolution and degradation that cellulose and lignin are inhibited while hemicellulose dissolution during taking, to obtain macromolecule
The hemicellulose of amount, high yield pulp1.Separation method through the invention, hemicellulose yield are 38.44-46.00%, wherein
The hemicellulose of 63.18-93.39% exists in the form of glycan, and cellulose yield is 10.36-18.69%, and lignin yield is
15.02-27.16%.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
The one or more aspects of invention have a thorough explanation, also may be implemented even without these specific details of the invention
These aspects.
Material equipment used in the present invention can be bought on the market；Wherein the reactor used in the present invention is six rotations
Turn reactor, is purchased from U.S. Greenwood company.
Embodiment 1
(1) by bamboo wood cutting at the small bamboo chip of 20-40mm long, 3-5mm wide, placement is dried at 105 DEG C absolutely in an oven
It is dry, it then collects spare；It takes 50g over dry bamboo chip to be put into reactor, distilled water, the weight ratio of over dry bamboo chip and distilled water is added
For 1:5, from room temperature to 145 DEG C of maximum temperature, heating-up time 60min, soaking time 60min under maximum temperature,
Extract is obtained, preconditions extract pH value using acetate buffer solution, so that extract final ph is 3, then keeps the temperature 60min
Afterwards, reactor is rinsed with cold water, reduces extract temperature, terminated reaction and carry out, liquid to be extracted is down to room temperature, filter is collected by filtration
Liquid；
(2) filtrate in (1) is taken, with the revolution of 5000rpm, clear liquid is collected after being centrifuged 10min under normal pressure, then adds 3 times
The ethanol solution that the mass fraction of volume is 95%, sufficiently miscible rear stratification, collects upper layer of extraction liquid, repeats to extract
3 times, be freeze-dried in the environment of -60 DEG C after extract liquor rotary evaporation, i.e., acquisition high molecular weight, high yield pulp1 hemicellulose.
It is 40.05% using the hemicellulose yield that this method obtains, wherein 78.89% hemicellulose sample is with glycan
Form exists, and cellulose yield is 15.59%, and lignin yield is 18.52%.
Embodiment 2
(1) by bamboo wood cutting at the small bamboo chip of 20-40mm long, 3-5mm wide, placement is dried at 105 DEG C absolutely in an oven
It is dry, it then collects spare；It takes 50g over dry bamboo chip to be put into reactor, distilled water, the weight ratio of over dry bamboo chip and distilled water is added
For 1:5, from room temperature to 170 DEG C of maximum temperature, heating-up time 60min, soaking time 60min under maximum temperature,
Extract is obtained, preconditions extract pH value using acetate buffer solution, so that extract final ph is 4, then keeps the temperature 60min
Afterwards, reactor is rinsed with cold water, reduces extract temperature, terminated reaction and carry out, liquid to be extracted is down to room temperature, filter is collected by filtration
Liquid；
(2) filtrate in (1) is taken, with the revolution of 5000rpm, clear liquid is collected after being centrifuged 10min under normal pressure, then adds 3 times
The ethanol solution that the mass fraction of volume is 95%, sufficiently miscible rear stratification, collects upper layer of extraction liquid, repeats to extract
3 times, be freeze-dried in the environment of -60 DEG C after extract liquor rotary evaporation, i.e., acquisition high molecular weight, high yield pulp1 hemicellulose.
It is 46.00% using the hemicellulose yield that this method obtains, wherein 93.39% hemicellulose sample is with glycan
Form exists, and cellulose yield is 10.36%, and lignin yield is 15.02%.
Embodiment 3
(1) by bamboo wood cutting at the small bamboo chip of 20-40mm long, 3-5mm wide, placement is dried at 105 DEG C absolutely in an oven
It is dry, it then collects spare；It takes 50g over dry bamboo chip to be put into reactor, distilled water, the weight ratio of over dry bamboo chip and distilled water is added
For 1:5, from room temperature to 160 DEG C of maximum temperature, heating-up time 60min, soaking time 60min under maximum temperature,
Extract is obtained, preconditions extract pH value using acetate buffer solution, so that extract final ph is 5；After keeping the temperature 60min,
Reactor is rinsed with cold water, reduces extract temperature, reaction is terminated and carries out, liquid to be extracted is down to room temperature, filtrate is collected by filtration；
(2) filtrate in (1) is taken, with the revolution of 5000rpm, clear liquid is collected after being centrifuged 10min under normal pressure, then adds 3 times
The sufficiently miscible rear stratification of the ethanol solution that the mass fraction of volume is 95%, collects upper layer of extraction liquid, repeats extraction 3
It is secondary, it is freeze-dried in the environment of -60 DEG C after extract liquor rotary evaporation, that is, obtains the hemicellulose of high molecular weight, high yield pulp1.
It is 38.44% using the hemicellulose yield that this method obtains, wherein 63.18% hemicellulose sample is with glycan
Form exists, and cellulose yield is 18.69%, and lignin yield is 27.16%.
Embodiment 4
(1) by bamboo wood cutting at the small bamboo chip of 20-40mm long, 3-5mm wide, placement is dried at 105 DEG C absolutely in an oven
It is dry, it then collects spare；It takes 50g over dry bamboo chip to be put into reactor, distilled water, the weight ratio of over dry bamboo chip and distilled water is added
For 1:4, from room temperature to 160 DEG C of maximum temperature, heating-up time 30min, soaking time 120min under maximum temperature,
Extract is obtained, preconditions extract pH value using acetate buffer solution, so that extract final ph is 4；After keeping the temperature 30min,
Reactor is rinsed with cold water, reduces extract temperature, reaction is terminated and carries out, liquid to be extracted is down to room temperature, filtrate is collected by filtration；
(2) filtrate in (1) is taken, with the revolution of 4500rpm, clear liquid is collected after being centrifuged 12min under normal pressure, then adds 2.5
Stratification after the ethanol solution that the mass fraction of times volume is 95% is sufficiently miscible, collects upper layer of extraction liquid, repeats to extract
It takes 3 times, is freeze-dried in the environment of -60 DEG C after extract liquor rotary evaporation, is i.e. acquisition high molecular weight, the hemicellulose of high yield pulp1
Element.
It is 42.14% using the hemicellulose yield that this method obtains, wherein 59.76% hemicellulose sample is with glycan
Form exists, and cellulose yield is 17.23%, and lignin yield is 23.20%.
Embodiment 5
(1) by bamboo wood cutting at the small bamboo chip of 20-40mm long, 3-5mm wide, placement is dried at 105 DEG C absolutely in an oven
It is dry, it then collects spare；It takes 50g over dry bamboo chip to be put into reactor, distilled water, the weight ratio of over dry bamboo chip and distilled water is added
For 1:7, from room temperature to 160 DEG C of maximum temperature, heating-up time 120min, soaking time 30min under maximum temperature,
Extract is obtained, preconditions extract pH value using acetate buffer solution, so that extract final ph is 4；After keeping the temperature 120min,
Reactor is rinsed with cold water, reduces extract temperature, reaction is terminated and carries out, liquid to be extracted is down to room temperature, filtrate is collected by filtration；
(2) filtrate in (1) is taken, with the revolution of 5200rpm, clear liquid is collected after being centrifuged 8min under normal pressure, then adds 3.5 times
The sufficiently miscible rear stratification of the ethanol solution that the mass fraction of volume is 95%, collects upper layer of extraction liquid, repeats extraction 3
It is secondary, it is freeze-dried in the environment of -60 DEG C after extract liquor rotary evaporation, that is, obtains the hemicellulose of high molecular weight, high yield pulp1.
It is 40.06% using the hemicellulose yield that this method obtains, wherein 62.16% hemicellulose sample is with glycan
Form exists, and cellulose yield is 15.43%, and lignin yield is 26.24%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method that bamboo hemicellulose efficiently separates, it is characterised in that: the following steps are included:
(1) by bamboo wood cutting at small bamboo chip, placement is dried to over dry at 105 DEG C in an oven, then collects spare；
(2) the small bamboo chip after weighing over dry is put into reactor, distilled water is added, and be heated to 145-170 DEG C, is then kept the temperature
0.5-2h obtains extract；The pH to 3-5 for adjusting extract again continues to stop reaction after keeping the temperature 0.5-2h；
(3) after liquid to be extracted is cooled to room temperature, filtrate is collected in filtering；
(4) clear liquid is collected after centrifugation in filtrate, ethanol solution is then added, sufficiently miscible rear stratification collects upper layer
Extract liquor repeats extraction 3 times, is freeze-dried after extract liquor rotary evaporation in the environment of -60 DEG C to get the hemicellulose.
2. the method that bamboo hemicellulose according to claim 1 efficiently separates, it is characterised in that: described in step (1)
The small a length of 20-40mm of bamboo chip, width 3-5mm.
3. the method that bamboo hemicellulose according to claim 1 efficiently separates, it is characterised in that: described in step (2)
The weight ratio of small bamboo chip and distilled water after over dry is 1:4-7.
4. the method that bamboo hemicellulose according to claim 1 efficiently separates, it is characterised in that: described in step (2)
The time of heating is 0.5-1.5h.
5. the method that bamboo hemicellulose according to claim 4 efficiently separates, it is characterised in that: in step (2), use
Acetate buffer solution adjusts the pH of the extract.
6. the method that bamboo hemicellulose according to claim 5 efficiently separates, it is characterised in that: described in step (4)
The revolving speed of centrifugation is 4500-5200rpm, and is centrifuged 8-12min under normal pressure.
7. the method that bamboo hemicellulose according to claim 5 efficiently separates, it is characterised in that: described in step (4)
Ethanol solution is 2.5-3.5 times of the supernatant volume, and the mass fraction of the dehydrated alcohol is 95%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110924206A (en) * | 2019-12-11 | 2020-03-27 | 国际竹藤中心 | Method for cleanly separating bamboo raw material components |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774478A (en) * | 2014-02-07 | 2014-05-07 | 福建农林大学 | Method of removing hemicelluloses by intensifying bamboo pre-hydrolysis by use of oxalic acid |
| CN103924468A (en) * | 2014-05-16 | 2014-07-16 | 长春工业大学 | Separation method of lignocellulose raw material ingredients |
| CN104153229A (en) * | 2014-07-16 | 2014-11-19 | 华南理工大学 | Preparation method of bamboo dissolving pulp |
| CN106011199A (en) * | 2016-07-19 | 2016-10-12 | 南京林业大学 | Method for pre-treating crop straw |
-
2018
- 2018-07-09 CN CN201810742645.0A patent/CN108951254A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774478A (en) * | 2014-02-07 | 2014-05-07 | 福建农林大学 | Method of removing hemicelluloses by intensifying bamboo pre-hydrolysis by use of oxalic acid |
| CN103924468A (en) * | 2014-05-16 | 2014-07-16 | 长春工业大学 | Separation method of lignocellulose raw material ingredients |
| CN104153229A (en) * | 2014-07-16 | 2014-11-19 | 华南理工大学 | Preparation method of bamboo dissolving pulp |
| CN106011199A (en) * | 2016-07-19 | 2016-10-12 | 南京林业大学 | Method for pre-treating crop straw |
Non-Patent Citations (1)
| Title |
|---|
| 朱宁等: "水热预水解分离相思木半纤维素及其组分与结构分析", 《化工学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110924206A (en) * | 2019-12-11 | 2020-03-27 | 国际竹藤中心 | Method for cleanly separating bamboo raw material components |
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