CN106186422A - A kind of method utilizing ultrafilter membrane to extract different molecular weight lignin - Google Patents
A kind of method utilizing ultrafilter membrane to extract different molecular weight lignin Download PDFInfo
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- CN106186422A CN106186422A CN201610633715.XA CN201610633715A CN106186422A CN 106186422 A CN106186422 A CN 106186422A CN 201610633715 A CN201610633715 A CN 201610633715A CN 106186422 A CN106186422 A CN 106186422A
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- lignin
- molecular weight
- ultrafilter membrane
- different molecular
- permeate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
- C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
Abstract
The invention discloses a kind of method utilizing ultrafilter membrane to extract different molecular weight lignin.The method uses the ultrafiltration membrane treatment black liquor of PSPP, then trapped fluid and permeate to obtaining carry out acid out process, it is settled out lignin, obtain the lignin of different molecular weight distribution, make lignin structure performance more homogeneous, be then oriented trans-utilization for without activity group content in fraction lignin.Extracting method according to the present invention utilizes ultrafiltration to obtain the lignin of different molecular weight distribution, and the lignin molecule amount size distribution obtained is narrow, the most homogeneous, simple to operate, and less energy intensive, comprehensive production cost is low.
Description
Technical field
The invention belongs to lignin separation field, be directed to a kind of utilize ultrafilter membrane to extract different molecular weight lignin
Method.
Background technology
The heavy polluted industry of paper industry Shi Shi China, is wherein mainly derived from paper waste, and black liquor of pulp making accounts for papermaking
The 80% of industrial wastewater discharge.According to incompletely statistics, the content about 3000 of lignin in China's paper industry black liquor of pulp making
Ten thousand tons, from black liquor, therefore reclaim lignin not only solve waste water pollution problem, and industrial emissions are turned waste into wealth, real
The efficient utilization of existing biomass resource, may advantageously facilitate sustainable development.More of that it is the most straight for the utilization of lignin
Connecing and burn with the heat-energy losses during supplementary paper industry, the most a small amount of lignin is used for fertilizer, building, oil and change
Work field, the higher value application level being exactly lignin in brief is relatively low.
The lignin structure that separate sources and separation method obtain differs greatly, the crosslink density of lignin height, structure
In inhomogeneity and lignin, the difference of active functional group content limits the higher value application of lignin.The molecular weight of lignin
Difference, activity group content contained therein is the most different, therefore if able to by lignin according to molecular size range, functional group
Enrichment degree separates cleanly and efficiently, it is thus achieved that a series of lignin characteristic molecule groups that polydispersity reduces, reactivity improves,
This is the most necessary for the rationally application of different molecular weight lignin.
Summary of the invention
For existing lignin structure complexity heterogeneity problem, the present invention provides one to utilize ultrafilter membrane to extract difference point
Son amount lignin method, use PSPP ultrafiltration membrane treatment black liquor, then to obtain trapped fluid and pass through
Liquid carries out acid out process, is settled out lignin, it is thus achieved that the lignin of different molecular weight distribution, makes lignin structure performance more
Add homogeneous, be then oriented trans-utilization for without activity group content in fraction lignin.
According to an aspect of the invention, it is provided a kind of method utilizing ultrafilter membrane to extract different molecular weight lignin:
(1), after poplar sulfate pulping black liquor is removed by filtration large particulate matter, add in ultrafiltration apparatus, initially with
Molecular cut off be 10000 ultrafilter membrane carry out ultrafiltration, period is stirred continuously, and obtains trapped fluid A and permeate A1；Permeate A1
The ultrafilter membrane continuing to use molecular cut off to be 5000 carries out ultrafiltration, obtains trapped fluid B and permeate B1；Permeate continues to use
Molecular cut off be 1000 ultrafilter membrane carry out ultrafiltration, obtain trapped fluid C and permeate D.
(2) in the liquid A collected, B, C, D, add sulphuric acid respectively, under room temperature, the pH value of solution is adjusted to 1.5-2.0, and
It is stirred continuously, is then centrifuged for separating, it is thus achieved that the lignin of different component, is designated as A ', B ', C ', D ' respectively.
(3) the lignin component A ' obtained, B ', C ', D ' are carried out lyophilization, then utilize gel permeation chromatography to survey
The molecular weight of amount lignin, it is thus achieved that there is the lignin of different molecular weight distribution.
It is also preferred that the left in described step (1), taking the black liquor volume after filtration is 200ml, and mixing speed is 200-300rpm,
Ultrafiltration pressure is 0.2-0.4MPa.
It is also preferred that the left in described step (2), including: sulfuric acid concentration is 2mol/L, and temperature is 20-30 DEG C, and mixing time is 1-
2h, mixing speed is 300-500rpm.
The distribution of the different molecular weight lignin obtained is respectively 400-600Da, 600-1000Da, 1000-
2000Da and 2000-3000Da.
Beneficial effect
Extracting method according to the present invention utilizes ultrafiltration to obtain the lignin of different molecular weight distribution, the wood obtained
Quality molecular size range narrowly distributing, the most homogeneous, simple to operate, less energy intensive, comprehensive production cost is low.
Accompanying drawing explanation
Fig. 1 is the gel permeation chromatography figure of lignin component A '；
Fig. 2 is the gel permeation chromatography figure of lignin component B '；
Fig. 3 is the gel permeation chromatography figure of lignin component C '；
Fig. 4 is the gel permeation chromatography figure of lignin component D '.
Detailed description of the invention
Hereinafter, will be described in detail the present invention.Before doing so, it should be appreciated that in this specification and appended
Claims in the term that uses should not be construed as and be limited to general sense and dictionary meanings, and inventor should allowed
On the basis of suitably definition term is to carry out the principle of best interpretations, according to implication corresponding with the technical elements of the present invention and generally
Thought explains.Therefore, description presented herein, merely for the sake of the preferred embodiment of illustration purpose, is not intended to limit this
The scope of invention, it will thus be appreciated that in the case of without departing from the spirit and scope of the present invention, can be obtained it by it
His equivalents or improved procedure.
Following example are enumerated only as the example of embodiment of the present invention, and the present invention does not constitute any limit
System, it will be appreciated by those skilled in the art that without departing from the present invention essence and design in the range of amendment each fall within the present invention
Protection domain.
Embodiment 1
900g over dry poplar loads 10L vertical electrical heating digester, and alkali charge 24% is (with Na2O counts), sulphidity 25%,
Solid-to-liquid ratio 1:5, is warming up to 165 DEG C, heating-up time 1h, is incubated 2-3h.Black liquor is collected in reaction after terminating, then use filter paper mistake
Filter, removes the large particulate matter in black liquor.
Embodiment 2
(1) black liquor 200ml after filtering in Example 1, adds in ultrafiltration apparatus, initially with molecular cut off is
The ultrafilter membrane of 10000 carries out ultrafiltration, and period is stirred continuously, mixing speed 200-300rpm, and ultrafiltration pressure is 0.2-0.4MPa,
To trapped fluid A and permeate A1；The ultrafilter membrane that permeate A1 continues to use molecular cut off to be 5000 carries out ultrafiltration, is retained
Liquid B and permeate B1；Permeate B1 continue use molecular cut off be 1000 ultrafilter membrane carry out ultrafiltration, obtain trapped fluid C and
Permeate D.
(2) in the liquid A collected, B, C, D, the sulphuric acid of 2mol/L is added respectively, by the pH of solution at room temperature 20-30 DEG C
Value is adjusted to 1.5-2.0, and is stirred continuously 1-2h, be then centrifuged for separate, it is thus achieved that the lignin of different component, be designated as respectively A ', B ',
C’、D’。
(3) the lignin component A ' obtained, B ', C ', D ' are carried out lyophilization, then utilize gel permeation chromatography to survey
The molecular weight of amount lignin, it is thus achieved that there is the lignin of different molecular weight distribution.
Embodiment 3
The mensuration of lignin molecule amount, assay method is as follows: weighs 4mg acetylation lignin sample and is dissolved in 2ml chromatograph
In level oxolane, dissolution filter, enter PLgel Mixed-D (300 × 7.5mm, Agilent, the U.S.) chromatographic column and be analyzed,
Sample size is 10ul.Leacheate is chromatographic grade oxolane, flow velocity 1ml/min.
Component A ', the gel permeation chromatography figure of B ', C ' and D ' see that Fig. 1, Fig. 2, Fig. 3 and Fig. 4, result explanation use this respectively
Method can realize the fractionated of sulfate-reducing conditions, it is thus achieved that the lignin of different molecular weight distribution, isolated three kinds of wood
Quality component A ', the average weight-average molecular weight of B ', C ' and D ' be respectively 2640g/mol, 1119g/mol, 700g/mol and 574g/
mol。
By examples detailed above it can be seen that ultrafiltration and acid-precipitation method are combined and can obtain different molecular weight distribution
Lignin, and operating process is simple, equipment needed thereby and invest less, and comprehensive production cost is low.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention.Any technology people being familiar with this specialty
Member, in the range of without departing from technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or modification
For the Equivalent embodiments of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit of the foundation present invention
Any simple modification, equivalent variations and the modification being made above example, all still falls within the range of technical solution of the present invention.
Claims (4)
1. the method that ultrafilter membrane extracts different molecular weight lignin, said method comprising the steps of:
(1), after poplar sulfate pulping black liquor is removed by filtration large particulate matter, add in ultrafiltration apparatus, initially with retaining
Molecular weight be 10000 ultrafilter membrane carry out ultrafiltration, period is stirred continuously, and obtains trapped fluid A and permeate A1；Permeate A1 continues
The ultrafilter membrane using molecular cut off to be 5000 carries out ultrafiltration, obtains trapped fluid B and permeate B1；Permeate continues employing and retains
Molecular weight be 1000 ultrafilter membrane carry out ultrafiltration, obtain trapped fluid C and permeate D；
(2) respectively to the liquid A collected, B, C, D add sulphuric acid, under room temperature, the pH value of solution is adjusted to 1.5-2.0, and constantly
Stirring, is then centrifuged for separating, it is thus achieved that the lignin of different component, is designated as A ', B ', C ', D ' respectively；
(3) the lignin component A ' obtained, B ', C ', D ' are carried out lyophilization, then utilize gel permeation chromatography to measure wood
The molecular weight of quality, it is thus achieved that there is the lignin of different molecular weight distribution.
Ultrafilter membrane the most according to claim 1 extracts the method for different molecular weight lignin, it is characterised in that described step
(1), in, taking the black liquor volume after filtration is 200ml, and mixing speed is 200-300rpm, and ultrafiltration pressure is 0.2-0.4MPa.
Ultrafilter membrane the most according to claim 1 extracts the method for different molecular weight lignin, it is characterised in that described step
(2) in, described sulfuric acid concentration is 2mol/L, and temperature is 20-30 DEG C, and mixing time is 1-2h, and mixing speed is 300-500rpm.
Ultrafilter membrane the most according to claim 1 extracts the method for different molecular weight lignin, it is characterised in that obtain not
It is respectively 400-600Da, 600-1000Da, 1000-2000Da with molecular weight lignin component A ', B ', C ', the distribution of D '
And 2000-3000Da.
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| CN201610633715.XA CN106186422A (en) | 2016-08-04 | 2016-08-04 | A kind of method utilizing ultrafilter membrane to extract different molecular weight lignin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108951250A (en) * | 2017-05-18 | 2018-12-07 | 济宁明升新材料有限公司 | A method of the extracting and developing lignin from sulfate pulping alkaline boiling liquid |
| CN109659151A (en) * | 2019-01-17 | 2019-04-19 | 中南大学 | A method of different Carbon-based supercapacitor electrode materials are prepared by regulating and controlling lignin molecule amount |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145998A (en) * | 2013-03-15 | 2013-06-12 | 浙江捷发科技有限公司 | Method for preparing lignin by utilizing papermaking black liquid |
| CN103665371A (en) * | 2013-11-14 | 2014-03-26 | 天津北洋百川生物技术有限公司 | Method for refining polyglutamic acid in biologic fermentation broth by using ultrafiltration and nanofiltration techniques |
| CN104927067A (en) * | 2015-06-29 | 2015-09-23 | 南京林业大学 | Method of extracting lignins different in molecular weight from bamboo pulping black liquor |
| CN105696396A (en) * | 2016-03-24 | 2016-06-22 | 广西壮族自治区中国科学院广西植物研究所 | Method for recovering hemicellulose, lignin and alkaline liquor from hemicellulose extraction liquid by separating flow |
-
2016
- 2016-08-04 CN CN201610633715.XA patent/CN106186422A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145998A (en) * | 2013-03-15 | 2013-06-12 | 浙江捷发科技有限公司 | Method for preparing lignin by utilizing papermaking black liquid |
| CN103665371A (en) * | 2013-11-14 | 2014-03-26 | 天津北洋百川生物技术有限公司 | Method for refining polyglutamic acid in biologic fermentation broth by using ultrafiltration and nanofiltration techniques |
| CN104927067A (en) * | 2015-06-29 | 2015-09-23 | 南京林业大学 | Method of extracting lignins different in molecular weight from bamboo pulping black liquor |
| CN105696396A (en) * | 2016-03-24 | 2016-06-22 | 广西壮族自治区中国科学院广西植物研究所 | Method for recovering hemicellulose, lignin and alkaline liquor from hemicellulose extraction liquid by separating flow |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108951250A (en) * | 2017-05-18 | 2018-12-07 | 济宁明升新材料有限公司 | A method of the extracting and developing lignin from sulfate pulping alkaline boiling liquid |
| CN109659151A (en) * | 2019-01-17 | 2019-04-19 | 中南大学 | A method of different Carbon-based supercapacitor electrode materials are prepared by regulating and controlling lignin molecule amount |
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Application publication date: 20161207 |