CN105754121A - Preparation method of ultrathin wood-fiber film - Google Patents
Preparation method of ultrathin wood-fiber film Download PDFInfo
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- CN105754121A CN105754121A CN201610239044.9A CN201610239044A CN105754121A CN 105754121 A CN105754121 A CN 105754121A CN 201610239044 A CN201610239044 A CN 201610239044A CN 105754121 A CN105754121 A CN 105754121A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
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Abstract
The invention relates to a preparation method of an ultrathin wood-fiber film and belongs to the field of biological bae material development.The preparation method which is simple in process and low in production cost includes: using a planetary ball mill to perform ball milling treatment on wood-fiber raw materials, dissolving the wood-fiber raw materials after the ball milling treatment in a LiCl/DMSO solvent system with the mass percentage being 8%, performing magnetic stirring for 2-48 hours under room temperature until the wood-fiber raw materials dissolve completely and the solution is transparent; preparing a wood-fiber solution with the concentration being 0.1-2%, using a spin-coating method to coat the wood-fiber solution on the surface of a QCM sensor gold electrode, performing multiple replacement washing in water after the coated solution is naturally dried, and performing vacuum drying to obtain the ultrathin wood-fiber film 5-20 nanometers in thickness.
Description
Technical field
The invention belongs to functional living being plasma membrane development field, the preparation method relating generally to a kind of ultra-thin wood fiber film.
Background technology
With lignocellulose for raw material, prepare the biomass goods such as biological material, chemicals and biomass fuel through bioconversion and become the hot topic of research both at home and abroad, be oligosaccharide by enzyme hydrolysis by polysaccharide conversion in lignocellulose raw material or monosaccharide be bioconversion key technology.Difference due to the complexity of lignocellulose raw material structure and chemical composition, and the complexity of itself and cellulase system, the research of early stage is concentrated mainly on the substrate change of total sugar yield in enzyme hydrolysis process through certain pretreatment, but these methods can not directly detect the kinetics in enzyme hydrolysis process, particularly in the initial period of enzymatic hydrolysis reaction.QCM (QCM) is very sensitive quality testing instrument, and its certainty of measurement, can original position, combination between real-time detection substrate and cellulase and catalytic reaction by being coated with the qcm sensor of wood fiber film up to nanogram level.
QCM chip applies ultra-thin wood fiber film, is that application QCM directly studies the key technology of pheron absorption and enzyme hydrolysis on lignocellulose.Preparing ultrathin membrane most common method is Langmuir-Blodgett (LB) and spin-coating method.Lignin Film, cellulose membrane, lignin and cellulose double-component thin film have been developed that preparation.Schaub etc. adopt LB method to be anchored on QCM silicon chip by TMSC, namely obtain cellulose membrane after removing derivatization；Hoeger etc. adopt spin-coating method TMSC and acetylation lignin to be anchored on QCM gold plaque, namely obtain cellulose and lignin bicomponent film after removing derivatization.But these thin film are that it exists very big-difference with lignocellulose raw material script structure by going derivatization to prepare after dissolving spin coating with the lignin of derivatization and cellulose for raw material.
Summary of the invention
For the deficiencies in the prior art, lignocellulose raw material through ball milling is directly dissolved in LiCl/DMSO system by the present invention, it is deposited onto on qcm sensor gold chip by spin-coating method, thus preparing the new type functional biomass membrane that can be used for detecting performing enzyme hydrolysis on wood fiber raw material characteristic.
The technical solution adopted in the present invention is: the preparation method of a kind of ultra-thin wood fiber film, comprises the following steps:
(1) take a certain amount of lignocellulosic material, adopt microphyte pulverizer to be ground into powder；
(2) screen with standard screen, obtain more uniform wood fibre powder, through benzene-ethanolic extraction ungrease treatment, after vacuum drying, adopt planetary ball mill that powder is carried out ball milling；
(3) wood fibre powder is dissolved in the LiCl/DMSO solution system that mass fraction is 8%, under room temperature after magnetic agitation 2-48h, obtains the wood fibre solution that clarification is bright；
(4) preparing certain density wood fibre solution, draw 100 μ L wood fibre solution with microsyringe, dropwise drip in qcm sensor gold electrode surfaces, when solution is diffused in whole surface, spin coating prepares liquid film；
(5) after liquid film natural drying, in ultra-pure water, after washing by soaking wood fibre solvent, vacuum drying, obtain can be used for detecting the ultra-thin wood fiber film of performing enzyme hydrolysis on wood fiber raw material characteristic.
In the method process that patent of the present invention provides, the lignocellulose raw material described in step (1) includes all wood fiber biomass such as timber, wood flour, straw, phragmites communis, rice husk, corn cob, Pericarppium arachidis hypogaeae and bagasse.
In the method process that patent of the present invention provides, the standard screen described in step (2) is 40～80 orders, obtains more uniform wood fibre powder after screening.
In the method process that patent of the present invention provides, the Ball-milling Time described in step (2) is 1～4h, and rotational speed of ball-mill is 300～1200r/min.
In the method process that patent of the present invention provides, the wood fibre solution concentration of the preparation described in step (4) is 0.1～2%.
In the method process that patent of the present invention provides, the spincoating conditions described in step (4) is rotation 20～60s under the rotating speed of 2000～5000r/min, repeats 1～4 time.
In the method process that patent of the present invention provides, spin coating liquid film described in step (5) can anchor at qcm sensor gold electrode surfaces after Indoor Natural dries 2～3 days, it is placed in ultra-pure water, changing a water every 2h, (using 0.1mol/LAgNO until being removed completely by LiCl and DMSO3Aqueous assay is without Cl-), finally vacuum drying at 40～60 DEG C.
The medicine have the advantages that
1. lignocellulose dissolving method provided by the present invention uses microphyte pulverizer and planetary ball mill lignocellulose to be pulverized and ball milling pretreatment, adopt LiCl and DMSO mixed liquor not changing the accessibility making on the basis of lignocellulose raw material original structure to which increase solvent to lignocellulose, dissolved efficiency can be improve as solvent.
2, the lignocellulose raw material used due to the present invention belongs to environment-friendly natural material, safety non-toxic and fully biodegradable, both the biomass combined film of preparation will not be produced toxicity, and cause environment pollution without equipment is produced burn into, also can reduce cost of material.
3, due to the present invention use ball milling, disintegrating apparatus simply common, it is not necessary to add expensive equipment, therefore can realize functional wood fibre composite membrane preparation technology at low cost.
4, the composite membrane preparation method of detection performing enzyme hydrolysis on wood fiber raw material characteristic provided by the invention is simple, and technique is easily controlled and production cost is low.
5, biomass combined film prepared by the present invention belongs to high value added product.Can efficiently utilize wood fiber biomass resource, widen purposes, improve its use value.
Below in conjunction with accompanying drawing, the invention will be further described.
Accompanying drawing explanation
Fig. 1 spin-coating method filming technology figure
The flow chart of Fig. 2 spin-coating method masking
The configuration of surface of the ultra-thin poplar film of Fig. 3
The XPS analysis of Fig. 4 poplar film
Fig. 5 poplar film is in the change of enzyme hydrolysis process medium frequency
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, technical matters step, it is embodied as condition and material, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not paying creative work premise, broadly fall into the scope of protection of the invention.
The lignocellulose raw material of the present invention includes all wood fiber biomass such as timber, wood flour, straw, phragmites communis, rice husk, corn cob, Pericarppium arachidis hypogaeae and bagasse.Hereinafter, with poplar and wheat straw for lignocellulose raw material, it is embodied as illustrating to the present invention.
Embodiment 1
Qcm sensor gold plaque is first soaked in NH3·H2O∶H2O2∶H2In O (volume ratio is 1: 1: 5) mixed liquor, heating 5min in 75 DEG C of thermostat water baths, then deionized water rinsing is clean, then dries up standby with clean nitrogen.Last before use again with UV-ozone instrument (UVO) irradiation (intensity 28mW/cm2, wavelength 254nm) and 10min.
It is peeled into thin slice with poplar, then air-dry, it is cut into the wood chip of length and width, thickness 3cm, 2cm, 2mm respectively, mix homogeneously back balance moisture is standby.Adopting microphyte pulverizer to process poplar wood chip, collect the wood powder of 40～80 orders with standard screen, through benzene-ethanolic extraction defat, process 4h with planetary ball mill after vacuum drying, rotational speed of ball-mill is 600rpm, often runs 5min and rests 10min, to prevent sample overheated.Ball milling wood powder is directly dissolved in, through vacuum drying, the LiCl/DMSO dicyandiamide solution that concentration is 8%, then makes the wood fibre solution of 0.5%.
Standby qcm sensor gold plaque is placed in KW-4A type spin-coating instrument, the 100 μ LLiCl/DMSO poplar solution dissolved is drawn with microsyringe, dropwise drip in sensor surface, diffuse to after whole sensor surface until solution, 60s is rotated under the rotating speed of 3000r/min, repeat 2 times, prepare liquid film (see Fig. 1).Natural drying disposed within for liquid film can be anchored at chip surface after 2～3 days, be placed in ultra-pure water, change a water every 2h, until LiCl and DMSO removes completely (uses 0.1mol/LAgNO3Aqueous assay is without Cl-), finally at 40 DEG C, vacuum drying prepares the ultra-thin poplar wood fiber film (see Fig. 2) that thickness is 5～10nm.The ultra-thin poplar film prepared is characterized, as shown in Figure 3 and Figure 4 with atomic force microscope (AFM) and x-ray photoelectron spectroscopy (XPS).
Embodiment 2
Qcm sensor gold plaque is first soaked in NH3·H2O∶H2O2∶H2In O (volume ratio is 1: 1: 5) mixed liquor, heating 5min in 75 DEG C of thermostat water baths, then deionized water rinsing is clean, then dries up standby with clean nitrogen.Last before use again with UV-ozone instrument (UVO) irradiation (intensity 28mW/cm2, wavelength 254nm) and 10min.
After air-dry, the blade of 3～5cm it is cut into wheat straw.Adopting microphyte pulverizer to process wheat straw, collect the barley seeding food of 40～80 orders with standard screen, through benzene-ethanolic extraction defat, process 2h with planetary ball mill after vacuum drying, rotational speed of ball-mill is 600rpm, often runs 5min and rests 10min, to prevent sample overheated.Ball milling wheat straw is directly dissolved in, through vacuum drying, the LiCl/DMSO dicyandiamide solution that concentration is 8%, makes the wood fibre solution of 1%.
Standby qcm sensor gold plaque is placed in KW-4A type spin-coating instrument, the 100 μ LLiCl/DMSO wheat straw solution dissolved is drawn with microsyringe, dropwise drip in sensor surface, diffuse to after whole sensor surface until solution, 40s is rotated under the rotating speed of 3500r/min, repeat 3 times, prepare liquid film (see Fig. 1).Liquid film natural drying disposed within can anchor at chip surface after 2～3 days, is placed in ultra-pure water, changes a water every 2h, until LiCl and DMSO removes completely (uses 0.1mol/LAgNO3Aqueous assay is without Cl-), finally at 40 DEG C, vacuum drying prepares the ultra-thin wheat straw wood fiber film (see Fig. 2) that thickness is 5～10nm.
Embodiment 3
Qcm sensor gold plaque is first soaked in NH3·H2O∶H2O2∶H2In O (volume ratio is 1: 1: 5) mixed liquor, heating 5min in 75 DEG C of thermostat water baths, then deionized water rinsing is clean, then dries up standby with clean nitrogen.Last before use again with UV-ozone instrument (UVO) irradiation (intensity 28mW/cm2, wavelength 254nm) and 10min.
It is peeled into thin slice with poplar, then air-dry, it is cut into the wood chip of length and width, thickness about 3cm, 2cm, 2mm respectively, mix homogeneously back balance moisture.Then in homemade swinging electrical heating oil bath boiling vessel, green liquor pretreatment is carried out, method is for taking above-mentioned poplar wood chip, adding relative to total titratable alkali (TotalTitratableAlkali, the TTA) consumption of over dry poplar is that 24% (w/w, with Na2O counts), sulphidity is that 25% (w/w, with Na2O counts), solid-to-liquid ratio is 1: 4 (w/v), in 80 DEG C of oil baths after revolution dipping 30min, with the ramp of 1 DEG C/min to maximum temperature 160 DEG C, is incubated 1h.Centrifuge dehydration after the poplar starting material with water of green liquor pretreatment is cleaned, equilibrium water conten in sealing container.Processing the poplar after green liquor pretreatment with microphyte pulverizer, collect the wood powder of 40～80 orders with standard screen, process 1h with planetary ball mill after vacuum drying, rotational speed of ball-mill is 600rpm, often runs 5min and rests 10min, to prevent sample overheated.It is directly dissolved in the LiCl/DMSO solution system that concentration is 8% after the green liquor pretreatment poplar vacuum drying of ball milling, makes poplar solution after the green liquor pretreatment of 0.5%.
Standby qcm sensor gold plaque is placed in KW-4A type spin-coating instrument, with microsyringe draw 100 μ LLiCl/DMSO dissolve green liquor pretreatment after poplar solution, dropwise drip in sensor surface, diffuse to after whole sensor surface until solution, 60s is rotated under the rotating speed of 3000r/min, repeat 2 times, prepare liquid film (see Fig. 1).Natural drying disposed within for liquid film can be anchored at chip surface after 2～3 days, be placed in ultra-pure water, change a water every 2h, until LiCl and DMSO removes completely (uses 0.1mol/LAgNO3Aqueous assay is without Cl-), finally at 40 DEG C, vacuum drying prepares ultra-thin green liquor pretreatment poplar film (see Fig. 2) that thickness is 10～15nm.
Embodiment 4
The ultra-thin poplar film present invention prepared is placed in the QCM reaction block detecting system, design temperature is 40 DEG C, carrying out fundamental frequency scanning, record the frequency change of 3 frequencys multiplication simultaneously by being furnished with the computer of signal acquiring system, the thickness thus calculating ultra-thin poplar film is 5～10nm.In reaction block, pass into, with the flow of 0.1mL/min, the Acetic acid-sodium acetate buffer that pH value is 4.8, until baseline balance after, in reaction block, pass into 0.1mg/mL, pH value is 4.8 cellulase solution (CTec2, Novozymes Company provides), the frequency simultaneously recording 3 frequencys multiplication by being furnished with the computer of signal acquiring system changes and analyzes frequency signal response curve.By be coated with ultra-thin poplar film qcm sensor be applied in QCM technology study poplar film enzyme hydrolysis behavior (see Fig. 5), wherein Δ F is the frequency change in enzyme hydrolysis process of the qcm sensor of coating poplar film, and its quality with adsorption layer is negative correlation.Δ F declines and represents that the quality of adsorption layer increases, and namely cellulase is adsorbed on substrate；Δ F raise represent adsorption layer Mass lost, namely cellulose generation enzymatic hydrolysis reaction and be degraded.The enzyme hydrolysis process of poplar film can be divided into 3 stages: stage i is adsorption process, and cellulase is adsorbed on substrate surface；Phase il is hydrolytic process, and cellulose starts hydrolysis under the catalytic action of enzyme；Ii I-stage is that the absorption to enzyme of equilibrium process, cellulose hydrolysis and lignin reaches poised state.
Every technical staff's notice: although the present invention describes according to above-mentioned detailed description of the invention, but the invention thought of the present invention is not limited to that invention, the repacking of any utilization inventive concept, all will include in this patent scope of patent protection.
Claims (7)
1. the preparation method of a ultra-thin wood fiber film, it is characterised in that comprise the following steps:
(1) take a certain amount of lignocellulose raw material, adopt microphyte pulverizer to be ground into powder；
(2) screen with standard screen, obtain more uniform wood fibre powder, through benzene-ethanolic extraction ungrease treatment, after vacuum drying, adopt planetary ball mill that powder is carried out ball milling；
(3) wood fibre powder is dissolved in the LiCl/DMSO solution system that mass fraction is 8%, under room temperature after magnetic agitation 2-48h, obtains the wood fibre solution that clarification is bright；
(4) preparing certain density wood fibre solution, draw 100 μ L wood fibre solution with microsyringe, dropwise drip in qcm sensor gold electrode surfaces, when solution is diffused in whole surface, spin coating prepares liquid film；
(5) after liquid film natural drying, in ultra-pure water, after washing by soaking wood fibre solvent, vacuum drying, obtain can be used for detecting the ultra-thin wood fiber film of performing enzyme hydrolysis on wood fiber raw material characteristic.
2. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterised in that the lignocellulose raw material described in step (1) includes all wood fiber biomass such as timber, wood flour, straw, phragmites communis, rice husk, corn cob, Pericarppium arachidis hypogaeae and bagasse.
3. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterised in that the standard screen described in step (2) is 40～80 orders, obtains more uniform wood fibre powder after screening.
4. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterised in that the Ball-milling Time described in step (2) is 1～4h, rotational speed of ball-mill is 300～1200r/mim.
5. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterised in that the wood fibre solution concentration of the preparation described in step (4) is 0.1～2%.
6. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterised in that the spincoating conditions described in step (4) is rotation 20～60s under the rotating speed of 2000～5000r/min, repeats 1～4 time.
7. the preparation method according to a claim 1 ultra-thin wood fiber film, it is characterized in that the spin coating liquid film described in step (5) can anchor at qcm sensor gold electrode surfaces after Indoor Natural dries 2～3 days, it is placed in ultra-pure water, changing a water every 2h, (using 0.1mol/LAgNO until being removed completely by LiCl and DMSO3Aqueous assay is without Cl-), finally vacuum drying at 40～60 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109187957A (en) * | 2018-09-04 | 2019-01-11 | 南京林业大学 | A method of with lignin in-situ modification gold chip |
| CN109239182A (en) * | 2018-09-04 | 2019-01-18 | 南京林业大学 | A method of with cellulase in-situ modification gold chip |
| CN113547598A (en) * | 2021-07-01 | 2021-10-26 | 德华兔宝宝装饰新材股份有限公司 | Preparation method of ultrathin wood vibrating diaphragm |
| WO2024060960A1 (en) * | 2022-09-20 | 2024-03-28 | 南京林业大学 | Method for characterizing interaction force between lignin and cellulase |
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| CN103773054A (en) * | 2013-12-26 | 2014-05-07 | 南京林业大学 | Preparation method of wood fiber bio-based plastic |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187957A (en) * | 2018-09-04 | 2019-01-11 | 南京林业大学 | A method of with lignin in-situ modification gold chip |
| CN109239182A (en) * | 2018-09-04 | 2019-01-18 | 南京林业大学 | A method of with cellulase in-situ modification gold chip |
| CN109239182B (en) * | 2018-09-04 | 2021-02-09 | 南京林业大学 | Method for in-situ modification of gold chip by cellulase |
| CN113547598A (en) * | 2021-07-01 | 2021-10-26 | 德华兔宝宝装饰新材股份有限公司 | Preparation method of ultrathin wood vibrating diaphragm |
| WO2024060960A1 (en) * | 2022-09-20 | 2024-03-28 | 南京林业大学 | Method for characterizing interaction force between lignin and cellulase |
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