CN107043462A - A kind of method that utilization reversed-phase emulsion prepares nano lignin - Google Patents
A kind of method that utilization reversed-phase emulsion prepares nano lignin Download PDFInfo
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- CN107043462A CN107043462A CN201710376235.4A CN201710376235A CN107043462A CN 107043462 A CN107043462 A CN 107043462A CN 201710376235 A CN201710376235 A CN 201710376235A CN 107043462 A CN107043462 A CN 107043462A
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- 229920005610 lignin Polymers 0.000 title claims abstract description 76
- 239000000839 emulsion Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000012071 phase Substances 0.000 claims abstract description 74
- 239000003513 alkali Substances 0.000 claims abstract description 35
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 21
- 239000008346 aqueous phase Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 38
- 235000019198 oils Nutrition 0.000 claims description 38
- 238000002156 mixing Methods 0.000 claims description 33
- 238000002360 preparation method Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000010030 laminating Methods 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229920001131 Pulp (paper) Polymers 0.000 claims description 4
- 210000000481 breast Anatomy 0.000 claims description 4
- 101100478055 Dictyostelium discoideum cotC gene Proteins 0.000 claims description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 239000010902 straw Substances 0.000 claims description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 2
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 claims description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 241001330002 Bambuseae Species 0.000 claims description 2
- 101100478056 Dictyostelium discoideum cotE gene Proteins 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 230000001154 acute effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 4
- 239000002585 base Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- -1 methoxyl group Chemical group 0.000 description 1
- 231100001083 no cytotoxicity Toxicity 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Colloid Chemistry (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
A kind of method that utilization reversed-phase emulsion prepares nano lignin, lipophilic emulsifier is dissolved in oil-based solvent and prepares oil phase, hydrophilic emulsifier and alkali lignin are dissolved in water and prepare aqueous phase, then aqueous phase is added drop-wise in oil phase, and alkali lignin reversed-phase emulsion is prepared under being stirred vigorously；Dilute acid soln is added drop-wise in oil phase with vigorous stirring and prepares diluted acid reversed-phase emulsion, diluted acid reversed-phase emulsion is mixed with alkali lignin reversed-phase emulsion again, certain time is slowly stirred after well mixed, nano lignin is obtained after being finally demulsified, filtered, washed and being freeze-dried.The nano lignin size uniformity prepared using the present invention, particle diameter is in 100 150 nm, and present invention process flow is simple, and solution used is recyclable, to environment without negative effect, has a good application prospect.
Description
Technical field
The present invention relates to a kind of method for preparing nano lignin, nanometer is prepared using reversed-phase emulsion more particularly, to one kind
The method of lignin.
Background technology
Lignin is the most abundant renewable and biodegradable natural organic high-molecular in the world in addition to cellulose,
It is one of important base material of new bio sill.It is main containing substantial amounts of phenyl ring, hydroxyl, methoxyl group etc. in lignin molecule structure
Construction unit and group are wanted, makes lignin that there are special physicochemical properties.Alkali lignin as pulp and paper industry pair
Product, annual global yield has 70,000,000 tons, and 95% is used as fuel or is discharged with black liquor, and only 5% is used for
High value added product is produced, mainly including additive, dispersant, adhesive and surfactant.In recent years, with human society
Attention to resource and environment sustainable development, the exploitation of the renewable biomass resources such as lignin are gradually caused extensively
Concern.
Continuing to develop for nanometer technology provides a new way, nano lignin for lignin-base product high value added utilization
Grain possess bigger serface, antibacterial, with polymer substrate compatibility is good and the features such as no cytotoxicity, can promote nano lignin
Application in fields such as inorganic filler, organizational project, photocatalysis carrier and regenerative medicines.Chinese invention patent
CN105829406A、CN104497322A、CN102002165A、CN103145999A、CN105153720A、
CN105854936A, CN103275331A and CN103254452A have been utilized respectively the precipitation method, supercritical fluid technique, Static Spinning
The technologies such as silk technology, high pressure homogenizer method are prepared for nano lignin.But, the precipitation method, supercritical fluid method and electrostatic spinning
Nano lignin particle diameter prepared by method is uncontrollable, and the equipment cost of high pressure homogenizer method is high, and it is limited to a certain extent
Extensive use.
The content of the invention
The technical problem to be solved in the present invention be overcome the deficiencies in the prior art there is provided one kind operation it is simpler, cost compared with
Low utilization reversed-phase emulsion prepares the method for nano lignin, obtained nano lignin size tunable.
The technical scheme that the present invention solves the use of its technical problem is that a kind of utilization reversed-phase emulsion prepares nano lignin
Method, comprises the following steps：
（1）Lipophilic emulsifier is dissolved in oil-based solvent and prepares oil phase, the mass content for controlling lipophilic emulsifier in oil phase is
6%-10%；
（2）Alkali lignin and hydrophilic emulsifier are dissolved in water and prepare aqueous phase, the mass content for controlling alkali lignin in aqueous phase is
1%-15%, the mass content for controlling hydrophilic emulsifier in aqueous phase is 5%-10%；The alkali lignin is in terms of effective ingredient；
（3）Low whipping speed for 1000-1500r/min being stirred vigorously under, by step（2）The aqueous phase of preparation is added drop-wise to part step
Suddenly（1）In the oil phase of middle preparation, the mass ratio for controlling aqueous phase and oil phase is 1:1-5, continues with mixing speed 1000-1500r/
Min is stirred vigorously more than 28min, obtains alkali lignin reversed-phase emulsion；
（4）Low whipping speed for 1000-1500r/min being stirred vigorously under, dilute acid soln is added drop-wise to step（1）Middle preparation
In another part oil phase, the mass ratio for controlling dilute acid soln and oil phase is 1:1-3, continues with mixing speed 1000-1500r/min
More than 28min is stirred vigorously, diluted acid reversed-phase emulsion is obtained；
（5）By step（4）The diluted acid reversed-phase emulsion and step of middle preparation（3）The alkali lignin reversed-phase emulsion mixing of middle preparation（Afterwards
The PH of face control system just defines the addition of diluted acid reversed-phase emulsion）, it is stirred vigorously with mixing speed 1000-1500r/min
More than 9min, then more than 0.9h is slowly stirred with mixing speed 100-300r/min, the PH for controlling whole system is 5-6, obtains mixed
Close emulsion；
（6）By step（5）Gained mixed emulsion at 50-60 DEG C with mixing speed 100-300r/min be slowly stirred 28min with
Upper progress demulsification processing, de-laminating solvent is added after demulsification makes creaming of emulsion, control hierarchy solvent and step（5）Gained mixed emulsion
Mass ratio be 1:1-3, isolates oil phase, receives remaining aqueous mixture；
（7）By step（6）In obtain remaining aqueous mixture filtering after repeatedly wash, until cleaning solution PH into neutrality, it is cold
Freeze after dry 12-24h, obtain nano lignin.
Further, step（1）In, the lipophilic emulsifier is the one or more in SP80, SP60, SP65.
Further, step（1）In, the oil-based solvent includes one kind in white oil, hexamethylene, hexane, toluene, vegetable oil
Or it is a variety of.
Further, step（2）In, the alkali lignin is that wood pulp alkali lignin, Straw Pulp alkali lignin, bamboo pulp alkali are wooden
One or more in element.
Further, step（2）In, the hydrophilic emulsifier is in OP10, tween80, Myrj 45
It is one or more.
Further, step（4）In, the dilute acid soln is in sulfuric acid solution, hydrochloric acid solution, salpeter solution, phosphoric acid solution
One or more.Preferred mass concentration is 5-15% dilute acid soln.
Further, step（6）In, the de-laminating solvent be ether, carbon tetrachloride, chloroform, dichloroethanes in one kind or
It is a variety of.
The method that nano lignin is prepared using reversed-phase emulsion of the present invention, the nano lignin size uniformity of preparation, grain
Footpath is in 100-150nm, and present invention process flow is simple, and solution used is recyclable, to environment without negative effect, with good
Good application prospect.Gained nano lignin size tunable, be beneficial to promote its catalyst carrier, ion adsorbing material,
The application in the fields such as biomedicine.
Brief description of the drawings
Fig. 1 is the SEM figures of the nano lignin prepared in comparative example 1；
Fig. 2 is the SEM figures of the nano lignin prepared in embodiment 1；
Fig. 3 is the SEM figures of the nano lignin prepared in embodiment 2.
Embodiment
Below in conjunction with specific embodiment so that the present invention is explained in more detail.
In each embodiment, unless otherwise indicated, the mass concentration of diluted acid is 10%.The alkali lignin is referred to effectively
Composition.
Comparative example 1：
（1）10 grams of lipophilic emulsifier SP80 are dissolved in 90 grams of white oils and prepare oil phase；
（2）10 grams of wood pulp alkali lignins and 10 grams of hydrophilic emulsifier OP10 are dissolved in 80 grams of water and prepare aqueous phase；（3）Acutely stirring
Mix（Mixing speed 1000r/min）Under, by step（2）The 40 grams of aqueous phases prepared are added drop-wise to 80 grams of steps（1）The oil phase of middle preparation
In, continue to be stirred vigorously（Mixing speed 1000r/min）Alkali lignin reversed-phase emulsion is obtained after 30min；
（4）It is being stirred vigorously（Mixing speed 1000r/min）Under, 10 grams of dilute hydrochloric acid solutions are added drop-wise to 120 grams of steps（3）Prepare
Alkali lignin reversed-phase emulsion in, continue to be stirred vigorously（Mixing speed 1000r/min）It is slowly stirred after 30min（Mixing speed
100r/min）Emulsion, is then slowly stirred by 1h at 60 DEG C（Mixing speed 100r/min）30min carries out demulsification processing, breaks
130 grams of ether are added after breast makes creaming of emulsion, isolates oil phase, receives and filters and repeatedly wash after remaining aqueous mixture, directly
To the PH of cleaning solution into neutrality, nano lignin is obtained after being freeze-dried 14h.The Size Distribution of gained nano lignin is homogeneous,
Particle diameter is in 200-800nm, as shown in Figure 1.
Embodiment 1：
（1）10 grams of lipophilic emulsifier SP80 are dissolved in 90 grams of white oils and prepare oil phase；
（2）10 grams of wood pulp alkali lignins and 10 grams of hydrophilic emulsifier OP10 are dissolved in 80 grams of water and prepare aqueous phase；
（3）It is being stirred vigorously（Mixing speed 1000r/min）Under, by 40 grams of steps（2）The aqueous phase of preparation is added drop-wise to 80 grams of steps
（1）In the oil phase of middle preparation, continue to be stirred vigorously（Mixing speed 1000r/min）After 30min, the anti-phase breast of alkali lignin is obtained
Liquid；
（4）It is being stirred vigorously（Mixing speed 1000r/min）Under, 10 grams of dilute hydrochloric acid solutions are added drop-wise to 10 grams of steps（1）Middle system
In standby oil phase, continue to be stirred vigorously（Mixing speed 1000r/min）Watery hydrochloric acid reversed-phase emulsion is obtained after 30min；
（5）Again by 20 grams of steps（4）The watery hydrochloric acid reversed-phase emulsion of middle preparation and 120 grams of steps（3）The alkali lignin of middle preparation is anti-
Phase emulsion is mixed, and is stirred vigorously（Mixing speed 1000r/min）It is slowly stirred after 10min（Mixing speed 100r/min）1h, control
The PH of whole system processed is 6, obtains mixed emulsion；
（6）Then by step（5）140 grams of mixed emulsions of gained are slowly stirred at 50 DEG C（Mixing speed 100r/min）30min
Demulsification processing is carried out, 140 grams of ether are added after demulsification makes creaming of emulsion, de-laminating solvent and step（5）The matter of gained mixed emulsion
Amount is than being 1:1, oil phase is isolated, remaining aqueous mixture is received；
（7）By step（6）In obtain remaining aqueous mixture filtering after repeatedly wash, until cleaning solution PH into neutrality, it is cold
Nano lignin is obtained after freezing dry 14h.The size uniformity of gained nano lignin, particle diameter is in 100-150nm, as shown in Figure 2.
Embodiment 2：
（1）10 grams of lipophilic emulsifier SP60 are dissolved in 90 grams of hexamethylenes and prepare oil phase；
（2）10 grams of Straw Pulp alkali lignins and 10 grams of hydrophilic emulsifier tween80 are dissolved in 80 grams of water and prepare aqueous phase；
（3）It is being stirred vigorously（Mixing speed 1000r/min）Under, by 40 grams of steps（2）The aqueous phase of preparation is added drop-wise to 80 grams of steps
（1）In the oil phase of middle preparation, continue to be stirred vigorously（Mixing speed 1000r/min）After 30min, the anti-phase breast of alkali lignin is obtained
Liquid；
（4）It is being stirred vigorously（Mixing speed 1000r/min）Under, 10 grams of dilution heat of sulfuric acid are added drop-wise to 10 grams of steps（1）Middle system
In standby oil phase, continue to be stirred vigorously（Mixing speed 1000r/min）Dilute sulfuric acid reversed-phase emulsion is obtained after 30min；
（5）Again by step（4）The 20 grams of dilute sulfuric acid reversed-phase emulsions and 120 grams of steps of middle preparation（3）The alkali lignin of middle preparation is anti-
Phase emulsion is mixed, and is stirred vigorously（Mixing speed 1000r/min）It is slowly stirred after 10min（Mixing speed 100r/min）1h, control
The PH of whole system processed is 6, obtains mixed emulsion；
（6）By step（5）140 grams of mixed emulsions of gained are slowly stirred at 60 DEG C（Mixing speed 100r/min）30min is carried out
Demulsification is handled, and 140 grams of carbon tetrachloride are added after demulsification makes creaming of emulsion, isolates oil phase, receives remaining aqueous mixture；
（7）By step（6）In obtain remaining aqueous mixture filtering after repeatedly wash, until cleaning solution PH into neutrality, it is cold
Nano lignin is obtained after freezing dry 14h.The size uniformity of gained nano lignin, particle diameter is in 100-150nm, as shown in Figure 3.
Claims (9)
1. a kind of method that utilization reversed-phase emulsion prepares nano lignin, it is characterised in that comprise the following steps：
（1）Lipophilic emulsifier is dissolved in oil-based solvent and prepares oil phase；
（2）Alkali lignin and hydrophilic emulsifier are dissolved in water and prepare aqueous phase；
（3）By step（2）The aqueous phase of preparation is added drop-wise to part steps（1）In the oil phase of middle preparation, the anti-phase breast of alkali lignin is obtained
Liquid；
（4）Dilute acid soln is added drop-wise to step（1）In another part oil phase of middle preparation, diluted acid reversed-phase emulsion is obtained；
（5）By step（4）The diluted acid reversed-phase emulsion and step of middle preparation（3）The alkali lignin reversed-phase emulsion mixing of middle preparation, is obtained
Mixed emulsion；
（6）By step（5）Gained mixed emulsion carries out demulsification processing, and de-laminating solvent is added after demulsification makes creaming of emulsion, isolates
Oil phase, receives remaining aqueous mixture；
（7）By step（6）In obtain remaining aqueous mixture filtering after repeatedly wash, until cleaning solution PH into neutrality, it is cold
It is lyophilized it is dry after, obtain nano lignin.
2. the method that utilization reversed-phase emulsion according to claim 1 prepares nano lignin, it is characterised in that including following
Step：
（1）Lipophilic emulsifier is dissolved in oil-based solvent and prepares oil phase, the mass content for controlling lipophilic emulsifier in oil phase is
6%-10%；
（2）Alkali lignin and hydrophilic emulsifier are dissolved in water and prepare aqueous phase, the mass content for controlling alkali lignin in aqueous phase is
1%-15%, the mass content for controlling hydrophilic emulsifier in aqueous phase is 5%-10%；The alkali lignin is in terms of effective ingredient；
（3）Low whipping speed for 1000-1500r/min being stirred vigorously under, by step（2）The aqueous phase of preparation is added drop-wise to part step
Suddenly（1）In the oil phase of middle preparation, the mass ratio for controlling aqueous phase and oil phase is 1:1-5, continues with mixing speed 1000-1500r/
Min is stirred vigorously more than 28min, obtains alkali lignin reversed-phase emulsion；
（4）Under low whipping speed 1000-1500r/min being stirred vigorously, dilute acid soln is added drop-wise to step（1）Middle preparation it is another
In a part of oil phase, the mass ratio for controlling dilute acid soln and oil phase is 1:1-3, continues acute with mixing speed 1000-1500r/min
Strong stirring more than 28min, obtains diluted acid reversed-phase emulsion；
（5）By step（4）The diluted acid reversed-phase emulsion and step of middle preparation（3）The alkali lignin reversed-phase emulsion mixing of middle preparation, with
Mixing speed 1000-1500r/min is stirred vigorously more than 9min, then with mixing speed 100-300r/min be slowly stirred 0.9h with
On, the PH for controlling whole system is 5-6, obtains mixed emulsion；
（6）By step（5）Gained mixed emulsion at 50-60 DEG C with mixing speed 100-300r/min be slowly stirred 28min with
Upper progress demulsification processing, de-laminating solvent is added after demulsification makes creaming of emulsion, control hierarchy solvent and step（5）Gained mixed emulsion
Mass ratio be 1:1-3, isolates oil phase, receives remaining aqueous mixture；
（7）By step（6）In obtain remaining aqueous mixture filtering after repeatedly wash, until cleaning solution PH into neutrality, it is cold
Freeze after dry 12-24h, obtain nano lignin.
3. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that step
（1）In, the lipophilic emulsifier is the one or more in SP80, SP60, SP65.
4. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that step
（1）In, the oil-based solvent includes the one or more in white oil, hexamethylene, hexane, toluene, vegetable oil.
5. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that step
（2）In, the alkali lignin is the one or more in wood pulp alkali lignin, Straw Pulp alkali lignin, bamboo pulp alkali lignin.
6. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that described
Hydrophilic emulsifier is the one or more in OP10, tween80, Myrj 45.
7. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that step
（4）In, the dilute acid soln is the one or more in sulfuric acid solution, hydrochloric acid solution, salpeter solution, phosphoric acid solution.
8. the method that utilization reversed-phase emulsion according to claim 7 prepares nano lignin, it is characterised in that the diluted acid
Solution is the dilute acid soln that mass concentration is 5-15%.
9. the method that utilization reversed-phase emulsion according to claim 1 or 2 prepares nano lignin, it is characterised in that step
（6）In, the de-laminating solvent is the one or more in ether, carbon tetrachloride, chloroform, dichloroethanes.
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| CN109054045A (en) * | 2018-08-13 | 2018-12-21 | 南京工业大学 | A kind of preparation method of sub-micron lignin |
| CN109161032A (en) * | 2018-08-21 | 2019-01-08 | 上海昶法新材料有限公司 | A kind of extracting method of lignin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054045A (en) * | 2018-08-13 | 2018-12-21 | 南京工业大学 | A kind of preparation method of sub-micron lignin |
| CN109054045B (en) * | 2018-08-13 | 2021-05-07 | 南京工业大学 | Preparation method of submicron lignin |
| CN109161032A (en) * | 2018-08-21 | 2019-01-08 | 上海昶法新材料有限公司 | A kind of extracting method of lignin |
| CN109161032B (en) * | 2018-08-21 | 2021-01-26 | 上海昶法新材料有限公司 | Method for extracting lignin |
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| CN107043462B (en) | 2019-04-26 |
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