CN104892970B - A kind of method that wood fibre directly prepares film forming - Google Patents
A kind of method that wood fibre directly prepares film forming Download PDFInfo
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- CN104892970B CN104892970B CN201510362860.4A CN201510362860A CN104892970B CN 104892970 B CN104892970 B CN 104892970B CN 201510362860 A CN201510362860 A CN 201510362860A CN 104892970 B CN104892970 B CN 104892970B
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- wood fibre
- ionic liquid
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Abstract
The invention provides a kind of method that wood fibre directly prepares film forming, its step are as follows：(1) ionic liquid is mixed with wood fibre, vacuum emulsifying shearing, wood fibre is dissolved in ionic liquid；(2) mixed solution is centrifuged, removes the gentle bubble of impurity, obtain wood fibre/ionic liquid homogeneous phase solution system；(3) supernatant after centrifugation is added in the mould for scribbling polytetrafluoroethylene (PTFE), horizontal rest, soaked after the basic coagulation forming of film liquid with deionized water, glycerine is uniformly then applied to surface is dried again.The method of the present invention requires no the pre-treatment of complexity, energy- and time-economizing, and the lignin and hemicellulose of reservation assign film feature, comprehensively make use of wood fibre.
Description
Technical field
The invention belongs to wood fibre manufacture field, and in particular to a kind of method that wood fibre directly prepares film forming.
Background technology
In recent years, as the deterioration of energy crisis and environmental problem, degradable biomaterial are increasingly taken seriously.Naturally
Fiber is gradually played an increasingly important role with the superior performance such as its light, degradable, inexpensive, high-modulus, high intensity.
To solve white pollution problems, researchers put forth effort on prepares various functions film, such as mulch film, preservative film using wood fibre
Deng.Due to the lignin in lignocellulosic components, hemicellulose and cellulose iii element are tightly combined, and are unfavorable for wood fibre dissolving
And film forming, so, the method generally used at present is to remove lignin and hemicellulose therein, is prepared into using cellulose
Film.
Some recent researchs show that the lignin and hemicellulose in some wood fibres also have certain feature,
For example the network structure that the lignin and hemicellulose of arghan interweave has antibiotic property.So retain therein wooden
Element and hemicellulose, not only eliminate the pre-treating technology of complicated and time consumption, can also strengthen the feature of film, also can be by wooden fibre
Dimension resource more fully and effectively develops.Therefore, finding a kind of method that wood fibre is directly prepared into film forming has pole
Big application value.
A kind of green solvent that has broad prospect of application of the ionic liquid as rising in recent years, have fixedness,
The advantages that good dissolubility and stability.But oil bath or microwave dissolve by heating technique, temperature is high, time length, consume energy compared with
Greatly, and wood fibre has a certain degree of degraded, limits its industrialized production.Therefore, from the emulsification of more energy-conserving and environment-protective
Shearing dissolution process is beneficial to the efficient utilization of fiber.
The content of the invention
The purpose of the present invention is to be directed to above technical problems to be solved, there is provided a kind of wood fibre prepares the side of film forming
Method, this method step is simple, and obtained film properties are good.
The technical solution of the present invention is as follows：
1. a kind of method that wood fibre directly prepares film forming, it is characterised in that step is as follows：
(1) ionic liquid is mixed with wood fibre, vacuum emulsifying shearing, wood fibre is dissolved in ion
In liquid；
(2) mixed solution is centrifuged, removes the gentle bubble of impurity, obtain wood fibre/ionic liquid homogeneous phase solution body
System；
(3) supernatant after centrifugation is added in the mould for scribbling polytetrafluoroethylene (PTFE), horizontal rest, film liquid is frozen into substantially
Soaked after type with deionized water, glycerine is uniformly then applied to surface is dried again.
Preferably, the ionic liquid be 1- butyl -3- methylimidazole villaumites, 1- pi-allyl -3- methylimidazole villaumites or
1- ethyl-3-methylimidazole acetate.
Preferably, it is pineapple flaxen fiber, bagasse or cotton fiber that the wood fibre, which includes but is not limited to,.
Preferably, the mass ratio of the wood fibre and ionic liquid is 2:100 to 10:100.
Preferably, in step (1), shear rate is 5000~26000rpm, and temperature is 40~150 DEG C；It is 2 to shear number
~15 times.
Preferably, in step (2), centrifuging temperature is normal temperature, and centrifugal speed is 3000~10000rpm, centrifugation time 10
~15 minutes.
Preferably, in step (3), normal temperature and pressure stand, time of repose be 4~6 hours, deionized water immersion time be
22-26 hours, depart to film from mould.
Preferably, temperature is unsuitable too high when drying, because moisture loss is too fast, the easy shrinkage of film, smearing glycerine can control
Moisture loss speed, it is effectively improved film problem of collapse.Preferably, in step (3), the glycerol concentration of smearing is 1-100%.
Preferably, in step (3), drying mode is vacuum drying or freeze-drying.
The method of the present invention has the advantages that：
1. dissolve wood fibre under the shearing force of vacuum emulsification homogenizer, so that its component will not drop
Solution, yield accordingly improve；
2. the preprocessor of complexity is required no, it is energy-efficient, and a certain degree of prevent soda acid and other materials
To wood fibre structural damage, obtained film properties are good；
3. realizing the technique that wood fibre is directly film-made, lignin and hemicellulose is utilized, assign film work(
Can property；
4. method is simple to operation, energy-conserving and environment-protective, meet the requirement of green production, be wood fibre film forming and follow-up synthesis
Using providing new thinking.
Embodiment
Technical scheme is described in further detail with reference to specific embodiment, but protection scope of the present invention
It is not limited in following examples.It should be noted that in view of length relation, following instance is only with pineapple fibre, bagasse, cotton
Exemplified by, illustrate method and step of the invention, but this method is equally applicable to other kinds of wood fibre, is not limited solely to described
And it is several.
Embodiment 1
2g arghans after crushing are added in 100g 1- butyl -3- methylimidazole villaumite ionic liquids, then
By vacuum homogeneous emulsifying machine, circulated 2 times under 100 DEG C, 16000rpm rotating speeds so that arghan is dissolved in ionic liquid
In, centrifuged using centrifuge under 4500rpm and remove within 10 minutes mixed liquor impurity and deaerate, obtain arghan/ionic liquid
Body homogeneous phase solution.Wood fibre determines after regeneration in solution, yield 95.4%.25g homogeneous phase solutions are weighed to pour into mould,
5 hours are stood after level, is soaked 24 hours with deionized water, is during which changed four water, be then uniformly applied to film with glycerite
Surface, after draining unnecessary glycerine, it is transferred to 40 DEG C of drying in baking oven.The glycerol concentration of smearing is 30%.The film for preparing gained is transparent
Uniformly, intensity is good, excellent in mechanical performance.
Embodiment 2
6g bagasse after crushing is added in 100g 1- pi-allyl -3- methylimidazole villaumite ionic liquids, Ran Houtong
Vacuum homogeneous emulsifying machine is crossed, is circulated 2 times under 80 DEG C, 18000rpm rotating speeds so that bagasse is dissolved in ionic liquid, is used
Centrifuge centrifuges 15 minutes under 4000rpm, removes impurity and deaerates, obtains bagasse fibre/ionic liquid homogeneous phase solution.It is molten
Wood fibre determines after regeneration in liquid, yield 90.3%.Weigh 25g homogeneous phase solutions to pour into mould, it is small to stand 6 after horizontal
When, soaked 24 hours with deionized water, during which change four water, film surface is then uniformly applied to glycerite, it is unnecessary to drain
After glycerine, 40 DEG C of drying in baking oven are transferred to.The glycerol concentration of smearing is 1%.The film clear homogeneous of gained is prepared, intensity is good, power
Learn excellent performance.
Embodiment 3
3g cotton fibers after crushing are added in 50g 1- pi-allyl -3- methylimidazole villaumite ionic liquids, then
By vacuum homogeneous emulsifying machine, being circulated 3 times under 80 DEG C, 15000rpm rotating speeds so that cotton fiber is dissolved in ionic liquid,
Centrifuged 15 minutes under 5000rpm using centrifuge, remove impurity and deaerate, obtain cotton fiber/ionic liquid homogeneous phase solution.
Wood fibre determines after regeneration in solution, yield 92.3%.Weigh 20g homogeneous phase solutions to pour into mould, 5 are stood after horizontal
Hour, soaked 24 hours with deionized water, during which change four water, film surface is then uniformly applied to glycerite, drain more
After emblic oil, 50 DEG C of drying in baking oven are transferred to.The glycerol concentration of smearing is 50%.The film clear homogeneous of gained is prepared, intensity is good,
Excellent in mechanical performance.
Embodiment 4
3g arghans after crushing are added in 100g 1- butyl -3- methylimidazole villaumite ionic liquids, then
By vacuum emulsification homogenizer machine, circulated 8 times under 60 DEG C, 5000rpm rotating speeds so that arghan is dissolved completely in ion
In liquid, centrifuged 10 minutes under 8000rpm using centrifuge, obtain arghan/ionic liquid homogeneous phase solution.In solution
Cellulose determines after regeneration, yield 92.0%.Weigh 25g homogeneous phase solutions to pour into mould, 4 hours are stood after horizontal, use
Deionized water is soaked 24 hours, during which changes four water, film surface is then uniformly applied to glycerite, drain unnecessary glycerine
Afterwards, 50 DEG C of drying in baking oven are transferred to.The glycerol concentration of smearing is 5%.The film clear homogeneous of gained is prepared, intensity is good, mechanical property
Can be excellent.
Embodiment 5
10g bagasse after crushing is added in 100g 1- butyl -3- methylimidazole villaumite ionic liquids, Ran Houtong
Vacuum emulsification homogenizer is crossed, is circulated 15 times under 150 DEG C, 26000rpm rotating speeds so that bagasse is dissolved completely in ionic liquid
In, centrifuged 10 minutes under 10000rpm using centrifuge, remove impurity and deaerate, it is equal to obtain bagasse fibre/ionic liquid
Phase solution.Wood fibre determines after regeneration in solution, yield 90.1%.30g homogeneous phase solutions are weighed to pour into mould, it is horizontal
5.5 hours are stood afterwards, is soaked 26 hours with deionized water, is during which changed four water, film table is then uniformly applied to glycerite
Face, after draining unnecessary glycerine, it is transferred to freeze drier drying.The glycerol concentration of smearing is 80%.The film for preparing gained is uniformly put down
Whole, intensity is good, excellent in mechanical performance.
Embodiment 6
2g cotton fibers after crushing are added in 100g 1- ethyl-3-methylimidazole acetate ionic liquids, then
By vacuum homogeneous emulsifying machine, circulated 10 times under 40 DEG C, 22000rpm rotating speeds so that cotton fiber is dissolved in ionic liquid
In, centrifuged at 3,000 rpm using centrifuge 15 minutes, remove impurity and deaerate, obtain cotton fiber/ionic liquid and mix
Liquid.Wood fibre determines after regeneration in solution, yield 91.3%.25g homogeneous phase solutions are weighed to pour into mould, it is quiet after horizontal
Put 4.5 hours, soaked 22 hours with deionized water, during which change four water, film surface is then uniformly applied to glycerite, drip
After removing unnecessary glycerine, 60 DEG C of drying in baking oven are transferred to.The glycerol concentration of smearing is 100%.The film clear homogeneous of gained is prepared, by force
Spend, excellent in mechanical performance.
Claims (9)
1. a kind of method that wood fibre directly prepares film forming, it is characterised in that step is as follows：
(1) ionic liquid is mixed with wood fibre, vacuum emulsifying shearing, wood fibre is dissolved in ionic liquid
In；
(2) mixed solution is centrifuged, removes the gentle bubble of impurity, obtain wood fibre/ionic liquid homogeneous phase solution system；
(3) supernatant after centrifugation is added in the mould for scribbling polytetrafluoroethylene (PTFE), horizontal rest, after the basic coagulation forming of film liquid
Soaked with deionized water, glycerine is uniformly then applied to surface is dried again.
2. according to the method for claim 1, it is characterised in that：The ionic liquid be 1- butyl -3- methylimidazole villaumites,
1- pi-allyl -3- methylimidazole villaumites or 1- ethyl-3-methylimidazole acetate.
3. according to the method for claim 1, it is characterised in that：The wood fibre is pineapple flaxen fiber, bagasse or cotton
Flower fiber.
4. according to the method for claim 1, it is characterised in that：The mass ratio of the wood fibre and ionic liquid is 2:
100 to 10:100.
5. according to the method for claim 1, it is characterised in that：In step (1), shear rate is 5000~26000rpm,
Temperature is 40~150 DEG C；It is 2~15 times to shear number.
6. according to the method for claim 1, it is characterised in that：In step (2), centrifuging temperature is normal temperature, and centrifugal speed is
3000~10000rpm, centrifugation time are 10~15 minutes.
7. according to the method for claim 1, it is characterised in that：In step (3), normal temperature and pressure stand, time of repose be 4~
6 hours, the time of deionized water immersion was 22-26 hours, is departed to film from mould.
8. according to the method for claim 1, it is characterised in that：In step (3), the glycerol concentration of smearing is 1-100%.
9. according to the method for claim 1, it is characterised in that：In step (3), drying mode is dry for vacuum drying or freezing
It is dry.
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| CN201510362860.4A CN104892970B (en) | 2015-06-26 | 2015-06-26 | A kind of method that wood fibre directly prepares film forming |
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| CN104892970B true CN104892970B (en) | 2018-03-30 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107400249B (en) * | 2017-07-26 | 2019-01-08 | 中国热带农业科学院海口实验站 | A kind of preparation method and applications of banana cellulose film |
| CN108396559A (en) * | 2018-02-05 | 2018-08-14 | 广西大学 | A kind of bagasse base film and preparation method thereof |
| CN109675530B (en) * | 2019-01-16 | 2020-01-10 | 南京林业大学 | Lignin phenol film paving method and prepared lignin phenol film |
| CN110078955B (en) * | 2019-03-29 | 2021-07-16 | 北京林业大学 | In-situ preparation method of xylose residue ultraviolet-resistant film, xylose residue ultraviolet-resistant film prepared by same and application thereof |
| CN111040449A (en) * | 2019-12-26 | 2020-04-21 | 合肥中汇睿能能源科技有限公司 | Modified polyimide film and preparation method thereof |
| CN112760976A (en) * | 2021-01-19 | 2021-05-07 | 谭旭鑫 | Xylem fiber with high toughness and preparation method thereof |
| CN114806205B (en) * | 2022-06-07 | 2023-06-20 | 西南交通大学 | Wood fiber-based film and preparation method and application thereof |
| CN116408860B (en) * | 2023-03-16 | 2024-03-12 | 广西大学 | Timber self-densification film and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164676A (en) * | 2007-08-22 | 2008-04-23 | 武汉大学 | Method for preparing cellulose gel film |
| CN101602865A (en) * | 2009-03-13 | 2009-12-16 | 王懋 | A kind of ethylcellulose mixed suspension liquid and preparation method thereof and application |
| CN101880411A (en) * | 2010-02-23 | 2010-11-10 | 广西壮族自治区化工研究院 | Method for preparing functionalized regenerated cellulose membranes by using bagasse celluloses |
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2015
- 2015-06-26 CN CN201510362860.4A patent/CN104892970B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164676A (en) * | 2007-08-22 | 2008-04-23 | 武汉大学 | Method for preparing cellulose gel film |
| CN101602865A (en) * | 2009-03-13 | 2009-12-16 | 王懋 | A kind of ethylcellulose mixed suspension liquid and preparation method thereof and application |
| CN101880411A (en) * | 2010-02-23 | 2010-11-10 | 广西壮族自治区化工研究院 | Method for preparing functionalized regenerated cellulose membranes by using bagasse celluloses |
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