CN107043462B - A method of nano lignin is prepared using reversed-phase emulsion - Google Patents
A method of nano lignin is prepared using reversed-phase emulsion Download PDFInfo
- Publication number
- CN107043462B CN107043462B CN201710376235.4A CN201710376235A CN107043462B CN 107043462 B CN107043462 B CN 107043462B CN 201710376235 A CN201710376235 A CN 201710376235A CN 107043462 B CN107043462 B CN 107043462B
- Authority
- CN
- China
- Prior art keywords
- phase
- reversed
- lignin
- emulsion
- phase emulsion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920005610 lignin Polymers 0.000 title claims abstract description 67
- 239000000839 emulsion Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003513 alkali Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 235000019198 oils Nutrition 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-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
- 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
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010030 laminating 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
- 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
- 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 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
- 229910017604 nitric acid Inorganic materials 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
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- 239000006210 lotion Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 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
- 239000002585 base Substances 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
- 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
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008187 granular material 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
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 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
- 239000000758 substrate Substances 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002023 wood 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
Landscapes
- 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 method of nano lignin is prepared using reversed-phase emulsion, lipophilic emulsifier is dissolved in oil-based solvent and prepares oily phase, hydrophilic emulsifier and alkali lignin are dissolved in water preparation water phase, then water phase is added drop-wise in oily phase, and alkali lignin reversed-phase emulsion is prepared under being vigorously stirred；Dilute acid soln is added drop-wise in oily 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, it is slowly stirred certain time after mixing, obtains nano lignin after being finally demulsified, filtered, washed and being freeze-dried.Prepared by the method nano lignin size uniformity, partial size is in 100-150 nm, and present invention process process 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 methods for preparing nano lignin, prepare nanometer using reversed-phase emulsion more particularly, to a kind of
The method of lignin.
Background technique
Lignin is the most abundant renewable and biodegradable natural organic high-molecular in the world in addition to cellulose,
It is one of the important substrate of new bio sill.It is main containing a large amount of phenyl ring, hydroxyl, methoxyl group etc. in lignin molecule structure
Structural unit and group are wanted, makes lignin that there are special physicochemical properties.Pair of the alkali lignin as pulp and paper industry
Product, annual global yield have 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 includes additive, dispersing agent, adhesive and surfactant.In recent years, with human society
Attention to resource and environment sustainable development, the development and utilization of the renewable biomass resources such as lignin gradually cause extensively
Concern.
The continuous development of nanotechnology provides a new way for lignin-base product high value added utilization, and nanometer is wooden
Crude granule possess bigger serface, antibacterial, with the features such as polymer substrate compatibility is good and no cytotoxicity, nano wood can be promoted
Application of the quality 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
The nano lignin partial size of method preparation is uncontrollable, and the equipment cost of high pressure homogenizer method is high, limits it to a certain extent
It is widely applied.
Summary of the invention
The technical problem to be solved by the present invention is to, overcome the deficiencies of the prior art and provide it is a kind of operation it is simpler, cost compared with
The low method using reversed-phase emulsion preparation nano lignin, obtained nano lignin size tunable.
The technical solution used to solve the technical problems of the present invention is that a kind of prepare nano lignin using reversed-phase emulsion
Method, comprising the following steps:
(1) lipophilic emulsifier is dissolved in oil-based solvent and prepares oily phase, the quality for controlling lipophilic emulsifier in oily phase contains
Amount is 6%-10%；
(2) alkali lignin and hydrophilic emulsifier are dissolved in water preparation water phase, the quality for controlling alkali lignin in water phase contains
Amount is 1%-15%, and the mass content for controlling hydrophilic emulsifier in water phase is 5%-10%；The alkali lignin is in terms of effective ingredient；
(3) under being vigorously stirred that low whipping speed is 1000-1500r/min, water phase prepared by step (2) is added drop-wise to portion
In the oily phase prepared in (1) step by step, the mass ratio of control water phase and oily phase is 1:1-5, is continued with mixing speed 1000-
1500r/min is vigorously stirred 28min or more, obtains alkali lignin reversed-phase emulsion；
(4) under being vigorously stirred that low whipping speed is 1000-1500r/min, dilute acid soln is added drop-wise to system in step (1)
In standby another part oil phase, the mass ratio of control dilute acid soln and oily phase is 1:1-3, is continued with mixing speed 1000-
1500r/min is vigorously stirred 28min or more, obtains diluted acid reversed-phase emulsion；
(5) the alkali lignin reversed-phase emulsion prepared in the diluted acid reversed-phase emulsion and step (3) that prepare in step (4) is mixed
(PH of back control system just defines the additional amount of diluted acid reversed-phase emulsion), is acutely stirred with mixing speed 1000-1500r/min
9min or more is mixed, then 0.9h or more is slowly stirred with mixing speed 100-300r/min, the PH for controlling whole system is 5-6, is obtained
Mixed emulsion；
(6) mixed emulsion obtained by step (5) is slowly stirred at 50-60 DEG C with mixing speed 100-300r/min
28min or more carries out demulsification processing, and de-laminating solvent is added after demulsification makes creaming of emulsion, control hierarchy solvent and step (5) gained
The mass ratio of mixed emulsion is 1:1-3, separates fuel-displaced phase, receives remaining aqueous mixture；
(7) it will repeatedly be washed after the filtering of residue aqueous mixture obtained in step (6), until the PH of cleaning solution is in
Property, after being freeze-dried 12-24h, obtain nano lignin.
Further, in step (1), the lipophilic emulsifier is one of SP80, SP60, SP65 or a variety of.
Further, in step (1), the oil-based solvent includes one of white oil, hexamethylene, hexane, toluene, vegetable oil
Or it is a variety of.
Further, in step (2), the alkali lignin is that wood pulp alkali lignin, Straw Pulp alkali lignin, bamboo pulp alkali are wooden
One of element is a variety of.
Further, in step (2), the hydrophilic emulsifier is OP10, tween80, in Myrj 45
It is one or more.
Further, in step (4), the dilute acid soln is sulfuric acid solution, in hydrochloric acid solution, nitric acid solution, phosphoric acid solution
It is one or more.Preferred mass concentration is the dilute acid soln of 5-15%.
Further, in step (6), the de-laminating solvent be one of ether, carbon tetrachloride, chloroform, dichloroethanes or
It is a variety of.
The method using reversed-phase emulsion preparation nano lignin of the present invention, the nano lignin size uniformity of preparation, grain
Diameter is in 100-150nm, and present invention process process is simple, and solution used is recyclable, to environment without negative effect, has good
Good application prospect.Gained nano lignin size tunable, be beneficial to push its catalyst carrier, ion adsorbing material,
The application in the fields such as biomedicine.
Detailed description of the invention
Fig. 1 is the SEM figure of the nano lignin prepared in comparative example 1；
Fig. 2 is the SEM figure of the nano lignin prepared in embodiment 1；
Fig. 3 is the SEM figure of the nano lignin prepared in embodiment 2.
Specific embodiment
Below in conjunction with specific embodiment the present invention is explained in more detail.
In each embodiment, unless otherwise stated, the mass concentration of diluted acid is 10%.The alkali lignin refers to effectively
Composition.
Comparative example 1:
(1) 10 grams of lipophilic emulsifier SP80 are dissolved in 90 grams of white oils and prepare oily phase；
(2) 10 grams of wood pulp alkali lignins and 10 grams of hydrophilic emulsifier OP10 are dissolved in 80 grams of water preparation water phases；(3) in play
Under strong stirring (mixing speed 1000r/min), 40 grams of water phases prepared by step (2) are added drop-wise to preparation in 80 grams of steps (1)
In oily phase, continue to obtain alkali lignin reversed-phase emulsion after being vigorously stirred (mixing speed 1000r/min) 30min；
(4) in the case where being vigorously stirred (mixing speed 1000r/min), 10 grams of dilute hydrochloric acid solutions are added drop-wise to 120 grams of steps (3)
In the alkali lignin reversed-phase emulsion of preparation, continue to be slowly stirred (stirring after being vigorously stirred (mixing speed 1000r/min) 30min
Speed 100r/min) 1h, then lotion is slowly stirred to (mixing speed 100r/min) 30min at 60 DEG C and carried out at demulsification
Reason, 130 grams of ether are added after demulsification makes creaming of emulsion, separates fuel-displaced phase, receives filtering and multiple water after remaining aqueous mixture
It washes, until the PH of cleaning solution obtains nano lignin after being freeze-dried 14h at neutrality.The size of gained nano lignin is distributed
Uniform, partial size 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 oily 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 water phase；
(3) in the case where being vigorously stirred (mixing speed 1000r/min), water phase prepared by 40 grams of steps (2) is added drop-wise to 80 grams
In the oily phase prepared in step (1), continues after being vigorously stirred (mixing speed 1000r/min) 30min, obtain alkali lignin reverse phase
Lotion；
(4) in the case where being vigorously stirred (mixing speed 1000r/min), 10 grams of dilute hydrochloric acid solutions are added drop-wise to 10 grams of steps (1)
In the oily phase of middle preparation, continue to obtain dilute hydrochloric acid reversed-phase emulsion after being vigorously stirred (mixing speed 1000r/min) 30min；
(5) again that the dilute hydrochloric acid reversed-phase emulsion prepared in 20 grams of steps (4) and the alkali prepared in 120 grams of steps (3) is wooden
Plain reversed-phase emulsion mixing, is slowly stirred (mixing speed 100r/min) after being vigorously stirred (mixing speed 1000r/min) 10min
1h, the PH for controlling whole system is 6, obtains mixed emulsion；
(6) 140 grams of mixed emulsions obtained by step (5) are then slowly stirred (mixing speed 100r/min) at 50 DEG C
30min carries out demulsification processing, and 140 grams of ether are added after demulsification makes creaming of emulsion, mixed emulsion obtained by de-laminating solvent and step (5)
Mass ratio be 1:1, separate fuel-displaced phase, receive remaining aqueous mixture；
(7) it will repeatedly be washed after the filtering of residue aqueous mixture obtained in step (6), until the PH of cleaning solution is in
Property, nano lignin is obtained after being freeze-dried 14h.The size uniformity of gained nano lignin, partial size is in 100-150nm, such as Fig. 2
It is shown.
Embodiment 2:
(1) 10 grams of lipophilic emulsifier SP60 are dissolved in 90 grams of hexamethylenes and prepare oily 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 water phase；
(3) in the case where being vigorously stirred (mixing speed 1000r/min), water phase prepared by 40 grams of steps (2) is added drop-wise to 80 grams
In the oily phase prepared in step (1), continues after being vigorously stirred (mixing speed 1000r/min) 30min, obtain alkali lignin reverse phase
Lotion；
(4) in the case where being vigorously stirred (mixing speed 1000r/min), 10 grams of dilution heat of sulfuric acid are added drop-wise to 10 grams of steps (1)
In the oily phase of middle preparation, continue to obtain dilute sulfuric acid reversed-phase emulsion after being vigorously stirred (mixing speed 1000r/min) 30min；
(5) again that the 20 grams of dilute sulfuric acid reversed-phase emulsions prepared in step (4) and the alkali prepared in 120 grams of steps (3) are wooden
Plain reversed-phase emulsion mixing, is slowly stirred (mixing speed 100r/min) after being vigorously stirred (mixing speed 1000r/min) 10min
1h, the PH for controlling whole system is 6, obtains mixed emulsion；
(6) 140 grams of mixed emulsions obtained by step (5) are slowly stirred (mixing speed 100r/min) 30min at 60 DEG C
Demulsification processing is carried out, 140 grams of carbon tetrachloride are added after demulsification makes creaming of emulsion, separates fuel-displaced phase, receives remaining aqueous mixture；
(7) it will repeatedly be washed after the filtering of residue aqueous mixture obtained in step (6), until the PH of cleaning solution is in
Property, nano lignin is obtained after being freeze-dried 14h.The size uniformity of gained nano lignin, partial size is in 100-150nm, such as Fig. 3
It is shown.
Claims (8)
1. a kind of method using reversed-phase emulsion preparation nano lignin, which comprises the following steps:
(1) lipophilic emulsifier is dissolved in oil-based solvent and prepares oily phase, the mass content for controlling lipophilic emulsifier in oily phase is
6%-10%；
(2) alkali lignin and hydrophilic emulsifier are dissolved in water preparation water phase, the mass content for controlling alkali lignin in water phase is
1%-15%, the mass content for controlling hydrophilic emulsifier in water phase is 5%-10%；The alkali lignin is in terms of effective ingredient；
(3) under being vigorously stirred that low whipping speed is 1000-1500r/min, water phase prepared by step (2) is added drop-wise to part step
Suddenly in the oily phase prepared in (1), the mass ratio of control water phase and oily phase is 1:1-5, is continued with mixing speed 1000-1500r/
Min is vigorously stirred 28min or more, obtains alkali lignin reversed-phase emulsion；
(4) under being vigorously stirred of low whipping speed 1000-1500r/min, dilute acid soln is added drop-wise to the another of the middle preparation of step (1)
In a part of oil phase, the mass ratio of control dilute acid soln and oily phase is 1:1-3, is continued acute with mixing speed 1000-1500r/min
Strong stirring 28min or more, obtains diluted acid reversed-phase emulsion；
(5) the alkali lignin reversed-phase emulsion prepared in the diluted acid reversed-phase emulsion and step (3) that prepare in step (4) is mixed, with
Mixing speed 1000-1500r/min is vigorously stirred 9min or more, 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 mixed emulsion obtained by step (5) at 50-60 DEG C with mixing speed 100-300r/min be slowly stirred 28min with
On carry out demulsification processing, de-laminating solvent is added after demulsification makes creaming of emulsion, mixed emulsion obtained by control hierarchy solvent and step (5)
Mass ratio be 1:1-3, separate fuel-displaced phase, receive remaining aqueous mixture；
(7) it will repeatedly be washed after the filtering of residue aqueous mixture obtained in step (6), until the PH of cleaning solution is at neutrality, it is cold
After dry 12-24h is lyophilized, nano lignin is obtained.
2. the method according to claim 1 using reversed-phase emulsion preparation nano lignin, which is characterized in that step (1)
In, the lipophilic emulsifier is one of SP80, SP60, SP65 or a variety of.
3. the method according to claim 1 or 2 using reversed-phase emulsion preparation nano lignin, which is characterized in that step
(1) in, the oil-based solvent includes one of white oil, hexamethylene, hexane, toluene, vegetable oil or a variety of.
4. the method according to claim 1 or 2 using reversed-phase emulsion preparation nano lignin, which is characterized in that step
(2) in, the alkali lignin is one of wood pulp alkali lignin, Straw Pulp alkali lignin, bamboo pulp alkali lignin or a variety of.
5. the method according to claim 1 or 2 using reversed-phase emulsion preparation nano lignin, which is characterized in that described
Hydrophilic emulsifier is one of OP10, tween80, Myrj 45 or a variety of.
6. the method according to claim 1 or 2 using reversed-phase emulsion preparation nano lignin, which is characterized in that step
(4) in, the dilute acid soln is one of sulfuric acid solution, hydrochloric acid solution, nitric acid solution, phosphoric acid solution or a variety of.
7. the method according to claim 6 using reversed-phase emulsion preparation nano lignin, which is characterized in that the diluted acid
Solution is the dilute acid soln that mass concentration is 5-15%.
8. the method according to claim 1 or 2 using reversed-phase emulsion preparation nano lignin, which is characterized in that step
(6) in, the de-laminating solvent is one of ether, carbon tetrachloride, chloroform, dichloroethanes or a variety of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710376235.4A CN107043462B (en) | 2017-05-25 | 2017-05-25 | A method of nano lignin is prepared using reversed-phase emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710376235.4A CN107043462B (en) | 2017-05-25 | 2017-05-25 | A method of nano lignin is prepared using reversed-phase emulsion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107043462A CN107043462A (en) | 2017-08-15 |
| CN107043462B true CN107043462B (en) | 2019-04-26 |
Family
ID=59546236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710376235.4A Active CN107043462B (en) | 2017-05-25 | 2017-05-25 | A method of nano lignin is prepared using reversed-phase emulsion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107043462B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054045B (en) * | 2018-08-13 | 2021-05-07 | 南京工业大学 | Preparation method of submicron lignin |
| CN109161032B (en) * | 2018-08-21 | 2021-01-26 | 上海昶法新材料有限公司 | Method for extracting lignin |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX270652B (en) * | 2001-12-07 | 2009-10-06 | Hercules Inc | ANIOIC COPOLYMERS PREPARED IN A REVERSE EMULSION MATRIX AND ITS USE WHEN PREPARING CELLULOSIC FIBER COMPOSITIONS. |
| CN103275331B (en) * | 2013-05-23 | 2015-08-12 | 广西大学 | A kind of take black liquid as the preparation method of the lignin nanoparticle of raw material |
| EP3080138B1 (en) * | 2013-12-12 | 2019-06-05 | Solenis Technologies, L.P. | Lignin nanoparticle dispersions and methods for producing and using the same |
| CN105153720B (en) * | 2015-09-30 | 2017-12-01 | 华南理工大学 | A kind of anti-phase nano-colloid ball of lignin and preparation method and application |
-
2017
- 2017-05-25 CN CN201710376235.4A patent/CN107043462B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107043462A (en) | 2017-08-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103866487B (en) | The preparation method of a kind of nano micro crystal cellulose/chitosan/polyvinyl alcohol composite nanometer film | |
| Zhu et al. | Towards sustainable production and utilization of plant-biomass-based nanomaterials: a review and analysis of recent developments | |
| CN105646721B (en) | A kind of preparation method of nano-cellulose fibril | |
| CN104136681B (en) | Method and apparatus for processing fibril cellulose and fibril cellulose product | |
| CN101070352B (en) | Method for preparing sheet-like microcrystal cellulose and modification processing method | |
| CN107043462B (en) | A method of nano lignin is prepared using reversed-phase emulsion | |
| CN102553470A (en) | Biological cellulose micro powder and application thereof | |
| CN109235102B (en) | Method for preparing cellulose nanofibrils through pretreatment of eutectic solvent | |
| CN103497476B (en) | Composite material based on amphoteric cellulose and application thereof | |
| CN105531419A (en) | A method of producing oxidized or microfibrillated cellulose | |
| CN112759772A (en) | Method for preparing Pickering emulsion from millet starch | |
| US20200308765A1 (en) | Method for producing parenchymal cell cellulose | |
| CN103242555A (en) | Acetylation lignin amphiphilic polymer nanometer colloid sphere and preparation method thereof | |
| CN107602709B (en) | Clean preparation method of carboxymethyl nano-cellulose material | |
| EP1753908A1 (en) | Method for producing a chemical conversion pulp | |
| CN110452396A (en) | A kind of preparation method of lignin micro-/ nano ball | |
| CN112267157A (en) | Preparation method of cellulose nano-fibrils modified based on reactive eutectic solvent | |
| JP7056987B1 (en) | Method for preparing amphipathic lignin nanomaterials from pulped black liquor, amphipathic lignin nanomaterials, sludge cleaner | |
| CN111303643B (en) | SiO of core-shell structure2@ paraffin nanoparticle and preparation method thereof | |
| CN102154936B (en) | Method for preparing paper making wet end chemical addition agent by using cassava residue as raw material | |
| CN111253970B (en) | Based on CO2/N2Preparation method of paraffin particles of switch emulsion and application of paraffin particles | |
| CN110684207B (en) | Nano micelle prepared by using lignosulfonate and preparation method thereof | |
| CN106186159B (en) | Adsorbing material for removing methylene blue in water and method for removing methylene blue in water by using adsorbing material | |
| CN108623817A (en) | A kind of green convenient method of the purifying lignin from raw alkaline lignin | |
| CN105970709B (en) | A method of isolating high purity cellulose from printing waste paper |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240409 Address after: Room 201, Office Building of Hunan Normal University Real Estate Management Office, No. 36 Lushan Road, Yuelu District, Changsha City, Hunan Province, 410006 Patentee after: Hunan Normal University Asset Management Co.,Ltd. Country or region after: China Address before: 410081 No. 36, Mount Lu, Changsha, Hunan, Yuelu District Patentee before: HUNAN NORMAL University Country or region before: China |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240507 Address after: 410012 Room 235, Building 9, Science and Technology Creative Park, Yuelu Street, Yuelu Mountain University Science and Technology City, Changsha City, Hunan Province Patentee after: Hunan Normal University Chemical New Materials Research Institute Co.,Ltd. Country or region after: China Address before: Room 201, Office Building of Hunan Normal University Real Estate Management Office, No. 36 Lushan Road, Yuelu District, Changsha City, Hunan Province, 410006 Patentee before: Hunan Normal University Asset Management Co.,Ltd. Country or region before: China |
|
| TR01 | Transfer of patent right |