CN110453533A - A kind of method that nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter - Google Patents
A kind of method that nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter Download PDFInfo
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- CN110453533A CN110453533A CN201910641152.2A CN201910641152A CN110453533A CN 110453533 A CN110453533 A CN 110453533A CN 201910641152 A CN201910641152 A CN 201910641152A CN 110453533 A CN110453533 A CN 110453533A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F13/00—Making discontinuous sheets of paper, pulpboard or cardboard, or of wet web, for fibreboard production
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
- D21H11/18—Highly hydrated, swollen or fibrillatable fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/71—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes
- D21H17/72—Mixtures of material ; Pulp or paper comprising several different materials not incorporated by special processes of organic material
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/08—Filter paper
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Paper (AREA)
Abstract
The invention discloses the methods that a kind of nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter, specifically comprise the following steps: step 1, prepare the cellulose microfibril containing lignin；Step 2, the cellulose nanometer paper containing lignin is prepared according to the resulting cellulose microfibril containing lignin of step 1；Step 3, the cellulose nanometer paper for absorbing whole wave band ultraviolet is had according to the resulting cellulose nanometer paper preparation containing lignin of step 2.Filter made from this method can make cellulose nanometer paper absorb ultraviolet light in full band range.
Description
Technical field
The invention belongs to biomass photoelectricity technical field of nano material, are related to a kind of nanometer paper absorption Avobenzone preparation
The method of whole wave band ultraviolet filter.
Background technique
Cellulose is one of the most abundant biological material in nature source, wide, biodegradable, nontoxic with source,
The advantages that environmentally friendly.Cellulose nano-fibrous (Cellulose Nanofibrils, abbreviation CNFs) is a kind of green material, diameter
10~40nm, length are several microns, are formed by natural wooden fiber through chemistry and mechanical treatment.It is cellulose nano-fibrous have compared with
High intensity, rigidity (modulus can reach 138GPa), biggish specific surface area (can achieve 50m2/ g), extremely low thermal expansion system
Number (CTE, 0.1ppm/k, close to quartz).Film can be made up in CNFs of suction filtration technique, be also cellulose nanometer
Paper.It has many unique performances, including optical clear, thermal stability, flexibility, Optical haze, high mechanical strength and
Chemical modification ability is strong.Also just because of these characteristics, cellulose nanometer paper has a wide range of applications field, such as solar-electricity
Pond, UV barriers function material, Organic Light Emitting Diode (OLED) and supercapacitor.
The ultraviolet light of earth surface can be divided into UVA (320~400nm) according to the wavelength of light, UVB (290~320nm) and
UVC (200-290nm), wherein UVA is about 98%.In recent years, ultraviolet light has caused the concern of people to the harm of human body.It is long
Time, which is exposed under solar ultraviolet radiation, to damage skin surface, such as skin photoage or cutaneum carcinoma.Moreover it is ultraviolet
Line irradiation can cause commodity accelerated ageing so as to cause the variation of commodity nature.Currently, cellulose nanometer paper can not achieve to complete
The filtering of band ultraviolet, thus study it is a kind of with absorb whole wave band ultraviolet cellulose nanometer paper base material seem especially
It is important.
Summary of the invention
The object of the present invention is to provide a kind of nanometer papers to adsorb the method that Avobenzone prepares whole wave band ultraviolet filter,
Filter made from this method can make cellulose nanometer paper absorb ultraviolet light in full band range.
The technical scheme adopted by the invention is that a kind of nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter
Method, specifically comprise the following steps:
Step 1, the cellulose microfibril containing lignin is prepared；
Step 2, the cellulose nanometer containing lignin is prepared according to the resulting cellulose microfibril containing lignin of step 1
Paper；
Step 3, had according to the resulting cellulose nanometer paper preparation containing lignin of step 2 and absorb whole wave band ultraviolet
Cellulose nanometer paper.
The features of the present invention also characterized in that
The detailed process of step 1 are as follows:
Using poplar APMP as raw material, sample is extracted using organic solvent, then evaporates Extract
Drying, the sample after drying remove hemicellulose using 15~20%NaOH solution, obtain the cellulose sample containing lignin,
Then different time is handled to the cellulose sample containing lignin with sodium chlorite method, obtains the fiber for containing different lignin contents
Plain sample then will shear the suspension that 10~30min is configured to 0.5~3wt% containing the cellulose sample of different lignin contents,
Homogenization 15~40 times under 90~150MPa pressure, obtain the cellulose microfibril containing lignin.
Organic solvent is the benzene and ethyl alcohol mixed with 2:1 ratio in step 1.
The detailed process of step 2 are as follows:
Taking oven-dry weight is the cellulose microfibril containing lignin of 0.025~1g, and deionized water, which is added, keeps solution dispersion equal
It is even, it is subsequently poured into sand core Suction filtration device and is filtered, after deionized water has been filtered, by filter membrane and wet cellulose nanometer paper
It removes, then separately takes a filter membrane, wet cellulose nanometer paper is placed between two filter membranes, then places it in two again
Assembly is formed between filter paper, then, assembly is placed between the smooth glass plate that pressure is 3~30Kg, is done at room temperature
Dry 8~72 hours, obtain the cellulose nanometer paper containing lignin.
The detailed process of step 3 are as follows:
Avobenzone and polymethyl methacrylate are mixed with the ratio of 1~30:1, and are dissolved in n,N dimethylformamide
3~10 hours, uniform solution is formed, is then impregnated in the cellulose nanometer paper made from step 2 containing lignin uniform
20~60min in solution, is then dried at normal temperature, obtains with the cellulose nanometer paper for absorbing whole wave band ultraviolet.
The invention has the advantages that the present invention, by handling from top to bottom, is protected on the basis of plant fiber material
The original relationship of plant fibre components is hold, natural cellulose nanometer paper base ultraviolet absorption material is obtained.Specifically with poplar
The wooden alkaline hydrogen peroxide mechanical pulp is raw material, obtains the cellulose containing lignin using NaOH solution removal hemicellulose, utilizes
The processing of sodium chlorite nanofarad obtains the cellulose of different lignin contents, obtains different lignin contents by high-pressure homogeneous and suction filtration
Cellulose nanometer paper finally impregnates through Avobenzone/polymethyl methacrylate (PMMA) solution and obtains LPANP paper.LPANP paper
Not only there is in full band range good ultraviolet absorption ability, but also show high optical clarity and mist degree.
High Optical haze can postpone the path of light, improve the ultraviolet radiation absorption efficiency of LPANP paper.Therefore LPANP paper is in ultraviolet light
There is good application prospect in terms of filter, flexible optoelectronic part and sensor.
In addition, cellulosic material of the present invention is from a wealth of sources, and it is not only environmentally protective renewable, it is low in cost, and
And the cellulose microfibril effect suspension stabilization of preparation is not easy coagulation and preparation process is simple.Compared to traditional cellulose nanometer
Paper, LPANP paper realize the ultraviolet radiation absorption in full band range, can be used as a kind of ideal ultraviolet filter.
Detailed description of the invention
Fig. 1 is that a kind of nanometer paper absorption Avobenzone of the present invention prepares embodiment in the method for whole wave band ultraviolet filter
The transmitted spectrum of LPANP paper obtained in 200-800nm in 1~10；
Fig. 2 is that a kind of nanometer paper absorption Avobenzone of the present invention prepares embodiment in the method for whole wave band ultraviolet filter
The transmitted spectrum of L-nanopaper paper obtained in 200-800nm in 1~10.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of method that nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter of the present invention, specifically includes as follows
Step:
Step 1, the cellulose microfibril (LCNF) containing lignin is prepared, specifically:
Using poplar APMP as raw material, sample is extracted using organic solvent (benzene: ethyl alcohol 2:1), then
Extract is evaporated and is dried, the sample after drying removes hemicellulose using 15~20%NaOH solution, obtains containing lignin
Cellulose sample obtains the cellulose sample of different lignin contents then with sodium chlorite method processing different time (0.5~4h)
Cellulose sample containing different lignin contents is then configured to the suspension of 0.5~3wt% by product through 10~30min of high speed shear
Liquid, homogenization 15~40 times under 90~150MPa pressure obtain the cellulose microfibril (LCNF) containing lignin.
Step 2, the cellulose nanometer paper containing lignin is prepared according to the resulting cellulose microfibril containing lignin of step 1
(L-nanopaper), specifically:
Taking oven-dry weight is the cellulose microfibril containing lignin of 0.025~1g, and deionized water, which is added, keeps solution dispersion equal
It is even, it is subsequently poured into sand core (place a water system miillpore filter) Suction filtration device and is filtered, the pressure of vacuum pump is -0.1~
After deionized water has filtered, filter membrane and wet cellulose nanometer paper are removed by 0.04MPa, then separately take a filter membrane, will be wet
Cellulose nanometer paper is placed between two filter membranes, and then by it, (it refers to wet cellulose nanometer paper and two filter membranes again
The entirety of composition) it is placed between two filter paper and forms assembly, then, it is the smooth of 3~30Kg that assembly, which is placed in pressure,
(blotting paper is placed with) between glass plate, is dried at room temperature for 8~72 hours, and the cellulose nanometer paper containing lignin is finally removed
(L-nanopaper)。
Step 3, had according to the resulting cellulose nanometer paper preparation containing lignin of step 2 and absorb whole wave band ultraviolet
Cellulose nanometer paper (LPANP), specifically:
Avobenzone and polymethyl methacrylate (PMMA) are mixed with the ratio of 1~30:1 and are dissolved in N, N dimethyl
Formamide 3~10 hours, form uniform solution.Then the cellulose nanometer paper containing lignin is impregnated in uniform solution
20~60min.It will then make it dry, be obtained with the cellulose nanometer paper for absorbing whole wave band ultraviolet at normal temperature
(LPANP)。
Embodiment 1
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 15%NaOH solution, obtains containing wood
The cellulose sample of element.Then 0.5h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 17.14%.With
Sample is configured to the suspension of 0.5wt% through high speed shear 10min afterwards, homogenization 40 times, are contained under 90MPa pressure
Having lignin is 17.14% cellulose microfibril.
Step 2, taking step 1 sample oven-dry weight is 0.025g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand
Core (placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, will after deionized water has filtered
Filter membrane and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, so
It is placed on again between two filter paper afterwards.Then, assembly is placed between the smooth glass plate that pressure is 3Kg and (is placed with blotting
Paper), it is dried at room temperature for 72h.Finally remove the cellulose nanometer paper for being 17.14% containing lignin.
Step 3, Avobenzone 9g and polymethyl methacrylate (PMMA) 0.3g are weighed, n,N dimethylformamide is dissolved in
3h forms uniform solution.Then step 2 sample is impregnated in 20min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-17.14) for absorbing whole wave band ultraviolet.
Embodiment 2
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 18%NaOH solution, obtains containing wood
The cellulose sample of element.Then with sodium chlorite method processing different time (1h), the cellulose that lignin content is 14.71% is obtained
Sample.Sample is then configured to the suspension of 1wt% through high speed shear 20min, homogenization 30 times under 120MPa pressure,
Obtain the cellulose microfibril for being 14.71% containing lignin.
Step 2, taking step 1 sample oven-dry weight is 0.05g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand
Core (placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is 0.07MPa, will after deionized water has filtered
Filter membrane and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, so
It is placed on again between two filter paper afterwards.Then, assembly is placed between the smooth glass plate that pressure is 10Kg and (is placed with blotting
Paper), it is dried at room temperature for 48h.Finally remove the cellulose nanometer paper for being 14.71% containing lignin.
Step 3, Avobenzone 10g and polymethyl methacrylate (PMMA) 0.5g are weighed, n,N dimethylformamide is dissolved in
5h forms uniform solution.Then step 2 sample is impregnated in 30min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-14.71) for absorbing whole wave band ultraviolet.
Embodiment 3
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 20%NaOH solution, obtains containing wood
The cellulose sample of element.Then 2h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 7.32%.Then will
Sample is configured to the suspension of 3wt% through high speed shear 30min, homogenization 20 times under 130MPa pressure, obtains containing wood
The cellulose microfibril that element is 7.32%.
Step 2, taking step 1 sample oven-dry weight is 0.5g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is 0.04MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 20Kg and (is placed with blotting paper),
It is dried at room temperature for 20h.Finally remove the cellulose nanometer paper for being 7.32% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-7.32) for absorbing whole wave band ultraviolet.
Embodiment 4
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 15%NaOH solution, obtains containing wood
The cellulose sample of element.Then 3h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 4.90%.Then will
Sample is configured to the suspension of 2wt% through high speed shear 20min, homogenization 15 times under 150MPa pressure, obtains containing wood
The cellulose microfibril that element is 4.90%.
Step 2, taking step 1 sample oven-dry weight is 1g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 30Kg and (is placed with blotting paper),
It is dried at room temperature for for 24 hours.Finally remove the cellulose nanometer paper for being 4.90% containing lignin.
Step 3, Avobenzone 5g and polymethyl methacrylate (PMMA) 5g are weighed, n,N dimethylformamide is dissolved in
10h forms uniform solution.Then step 2 sample is impregnated in 60min in uniform solution.It will then be made at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-4.90) for absorbing full spectrum ultraviolet light.
Embodiment 5
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 18%NaOH solution, obtains containing wood
The cellulose sample of element.Then 4h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 1.27%.Then will
Sample is configured to the suspension of 3wt% through high speed shear 30min, homogenization 20 times under 130MPa pressure, obtains containing wood
The cellulose microfibril that element is 1.27%.
Step 2, taking step 1 sample oven-dry weight is 0.5g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 30Kg and (is placed with blotting paper),
It is dried at room temperature for for 24 hours.Finally remove the cellulose nanometer paper for being 1.27% containing lignin.
Step 3, Avobenzone 10g and polymethyl methacrylate (PMMA) 0.5g are weighed, n,N dimethylformamide is dissolved in
5h forms uniform solution.Then step 2 sample is impregnated in 30min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-1.27) for absorbing whole wave band ultraviolet.
Embodiment 6
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 15%NaOH solution, obtains containing wood
The cellulose sample of element.Then 0.5h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 17.14%.With
Sample is configured to the suspension of 0.5wt% through high speed shear 10min afterwards, homogenization 40 times, are contained under 90MPa pressure
Having lignin is 17.14% cellulose microfibril.
Step 2, taking step 1 sample oven-dry weight is 0.025g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand
Core (placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, will after deionized water has filtered
Filter membrane and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, so
It is placed on again between two filter paper afterwards.Then, assembly is placed between the smooth glass plate that pressure is 3Kg and (is placed with blotting
Paper), it is dried at room temperature for 72h.Finally remove the cellulose nanometer paper for being 17.14% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-17.14) for absorbing full spectrum ultraviolet light.
Embodiment 7
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 18%NaOH solution, obtains containing wood
The cellulose sample of element.Then 1h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 14.71%.Then
Sample is configured to the suspension of 1wt% through high speed shear 20min, homogenization 30 times, are contained under 120MPa pressure
The cellulose microfibril that lignin is 14.71%.
Step 2, taking step 1 sample oven-dry weight is 0.05g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand
Core (placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is 0.07MPa, will after deionized water has filtered
Filter membrane and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, so
It is placed on again between two filter paper afterwards.Then, assembly is placed between the smooth glass plate that pressure is 10Kg and (is placed with blotting
Paper), it is dried at room temperature for 48h.Finally remove the cellulose nanometer paper for being 14.71% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-14.71) for absorbing whole wave band ultraviolet.
Embodiment 8
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 20%NaOH solution, obtains containing wood
The cellulose sample of element.Then 2h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 7.32%.Then will
Sample is configured to the suspension of 3wt% through high speed shear 30min, homogenization 20 times under 130MPa pressure, obtains containing wood
The cellulose microfibril that element is 7.32%.
Step 2, taking step 1 sample oven-dry weight is 0.5g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is 0.04MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 20Kg and (is placed with blotting paper),
It is dried at room temperature for 20h.Finally remove the cellulose nanometer paper for being 7.32% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-7.32) for absorbing whole wave band ultraviolet.
Embodiment 9
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 15%NaOH solution, obtains containing wood
The cellulose sample of element.Then 3h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 4.90%.Then will
Sample is configured to the suspension of 2wt% through high speed shear 20min, homogenization 15 times under 150MPa pressure, obtains containing wood
The cellulose microfibril that element is 4.90%.
Step 2, taking step 1 sample oven-dry weight is 1g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 30Kg and (is placed with blotting paper),
It is dried at room temperature for for 24 hours.Finally remove the cellulose nanometer paper for being 4.90% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-4.90) for absorbing full spectrum ultraviolet light.
Embodiment 10
Step 1, it using poplar APMP as raw material, is extracted and is tried using organic solvent (benzene: ethyl alcohol 2:1)
Then Extract is evaporated and is dried by sample.Sample after drying removes hemicellulose using 18%NaOH solution, obtains containing wood
The cellulose sample of element.Then 4h is handled with sodium chlorite method, obtains the cellulose sample that lignin content is 1.27%.Then will
Sample is configured to the suspension of 3wt% through high speed shear 30min, homogenization 20 times under 130MPa pressure, obtains containing wood
The cellulose microfibril that element is 1.27%.
Step 2, taking step 1 sample oven-dry weight is 0.5g, and deionized water, which is added, makes solution be uniformly dispersed, and is subsequently poured into sand core
(placing a water system miillpore filter) Suction filtration device, the pressure of vacuum pump is -0.1MPa, after deionized water has filtered, will be filtered
Film and wet cellulose nanometer paper are removed, then are in wet cellulose nanometer paper between two filter membranes with a filter membrane, then
It is placed between two filter paper again.Then, assembly is placed between the smooth glass plate that pressure is 30Kg and (is placed with blotting paper),
It is dried at room temperature for for 24 hours.Finally remove the cellulose nanometer paper for being 1.27% containing lignin.
Step 3, Avobenzone 8g and polymethyl methacrylate (PMMA) 0.8g are weighed, n,N dimethylformamide is dissolved in
8h forms uniform solution.Then step 2 sample is impregnated in 40min in uniform solution.Then it will be made to do at normal temperature
It is dry, it obtains with the cellulose nanometer paper (LPANP-1.27) for absorbing whole wave band ultraviolet.
The ultraviolet (uv) transmission curve for the LPANP paper that Examples 1 to 10 obtains is as shown in Figure 1, as can be seen from the figure LPANP
Ultraviolet filter rate of the paper in the region UVC is higher than 95%, and the ultraviolet light in the region UVB is blocked more than the area 88%, Er UVA
The ultraviolet light in domain is almost blocked.Compared to L-nanopaper paper (as shown in Figure 2), LPANP paper shows good UV
(UVC, UVB and UVA) absorbent properties realize ultraviolet radiation absorption of the cellulose nanometer paper in full band range.
Claims (5)
1. a kind of method that nanometer paper absorption Avobenzone prepares whole wave band ultraviolet filter, it is characterised in that: specifically include
Following steps:
Step 1, the cellulose microfibril containing lignin is prepared；
Step 2, the cellulose nanometer paper containing lignin is prepared according to the resulting cellulose microfibril containing lignin of step 1；
Step 3, the fiber for absorbing whole wave band ultraviolet is had according to the resulting cellulose nanometer paper preparation containing lignin of step 2
Plain nanometer paper.
2. the method that a kind of nanometer paper absorption Avobenzone according to claim 1 prepares whole wave band ultraviolet filter,
It is characterized by: the detailed process of the step 1 are as follows:
Using poplar APMP as raw material, sample is extracted using organic solvent, then Extract is evaporated and is dried,
Sample after drying removes hemicellulose using 15~20%NaOH solution, obtains the cellulose sample containing lignin, then use
Sodium chlorite method handles different time to the cellulose sample containing lignin, obtains the cellulose sample for containing different lignin contents
Product then will shear the suspension that 10~30min is configured to 0.5~3wt% containing the cellulose sample of different lignin contents, 90
Homogenization 15~40 times, obtains the cellulose microfibril containing lignin under~150MPa pressure.
3. the method that a kind of nanometer paper absorption Avobenzone according to claim 2 prepares whole wave band ultraviolet filter,
It is characterized by: organic solvent is the benzene and ethyl alcohol mixed with 2:1 ratio in the step 1.
4. the method that a kind of nanometer paper absorption Avobenzone according to claim 1 prepares whole wave band ultraviolet filter,
It is characterized by: the detailed process of the step 2 are as follows:
Taking oven-dry weight is the cellulose microfibril containing lignin of 0.025~1g, and deionized water, which is added, makes solution be uniformly dispersed, so
After pour into sand core Suction filtration device and filtered, after deionized water has been filtered, filter membrane and wet cellulose nanometer paper are removed,
A filter membrane is separately taken again, wet cellulose nanometer paper is placed between two filter membranes, then places it in two filter paper again
Between form assembly, then, assembly is placed between the smooth glass plate that pressure is 3~30Kg, be dried at room temperature for 8~
72 hours, obtain the cellulose nanometer paper containing lignin.
5. the method that a kind of nanometer paper absorption Avobenzone according to claim 1 prepares whole wave band ultraviolet filter,
It is characterized by: the detailed process of the step 3 are as follows:
Avobenzone and polymethyl methacrylate are mixed with the ratio of 1~30:1, and be dissolved in n,N dimethylformamide 3~
10 hours, uniform solution is formed, the cellulose nanometer paper made from step 2 containing lignin is then impregnated in uniform solution
In 20~60min, be then dried at normal temperature, obtain with absorb whole wave band ultraviolet cellulose nanometer paper.
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