CN103388273A - Method for preparing nanometer hydrophobic paper by utilizing corrugated paper/nanometer titanium dioxide - Google Patents
Method for preparing nanometer hydrophobic paper by utilizing corrugated paper/nanometer titanium dioxide Download PDFInfo
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Abstract
The invention discloses a method for preparing nanometer hydrophobic paper by utilizing corrugated paper/nanometer titanium dioxide. The method specifically comprises three steps of: (1), chemically pretreating; (2), preparing nanometer cellulose by mechanical treatments including grinding and ultrasonically treating; and (3), compounding the prepared nanometer cellulose solution with the nanometer titanium dioxide, and preparing super-hydrophobic nanometer paper by adopting a vacuum suction filtration way under the normal temperature under the action of a silane coupling agent. The method for preparing nanometer hydrophobic paper by utilizing corrugated paper/nanometer titanium dioxide has the advantages that the nanometer paper with the titanium dioxide concentration of 10%, which is prepared by the method, has strength of 63MPa and a good hydrophobic effect. Moreover, the method is simple and easy to implement, simple to operate, small in device investment and capable of carrying out large-scale production.
Description
Technical field
What the present invention relates to is a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper.Belong to the biomass nano fibrous material.
Background technology
Titanium dioxide (TiO
2) be a kind of important inorganic semiconductor functional material, have wet sensitive, air-sensitive, dielectric effect, photoelectric conversion and the superior characteristics such as photocatalysis performance, in high-tech areas such as sensor, dielectric material, self-cleaning material, solar cell, photocatalytic degradation pollutants, important application prospect is arranged.
Nano titanium oxide has very strong " super-hydrophobicity ", be difficult for forming the globule on its surface, and nano titanium oxide can be to the hydrocarbon effect under radiation of visible light.Utilize a characteristic like this can be coated with on the surface of glass, pottery and ceramic tile last layer nano titanium oxide thin layer, utilize the light-catalyzed reaction of titanium oxide just can be decomposed into CO to the organic pollution that is adsorbed on titania surface
2And O
2, together can be clean by rain drop erosion with remaining inorganic matter, thus realize self-cleaning function.The existing people in Tokyo is at laboratory development success self-cleaning ceramic tile, the skim nano titanium oxide is arranged on the surface of this new product, any pickup material from the teeth outwards, comprise that greasy dirt, bacterium are under the irradiation of light,, due to the catalytic action of nano titanium oxide, can make the further oxidation of these hydrocarbon materials become gas or be easy to the material of being wiped.The nano titanium dioxide photocatalysis effect makes all become easy the keeping a public place clean etc. of ceramic tile, automobile rearview mirror and front screen of glass, the easy pickup in kitchen of skyscraper.
Fluting medium generally prepares ground wood pulp or semi-chemical pulp manufacturing with leaf wood, and is all better aspect the physical strengths such as deflection, ring crush intensity, TENSILE STRENGTH, bursting strength, tear-resistant degree, and the bulk of paper is better.
More botanic plant surfaces such as lotus leaf, paddy rice, rose, and the surfaces such as the special skin of some animals, claw itself are to the special hydrophobic effect of water droplet.This special surface texture can make plant surface keep the automatically cleaning on blade face, extend the time of staying of water droplet at plant surface, and the contact area that enlarges animal and water, thereby animal capable is stopped at the water surface safely, and the resistance that slows down water in animal movement.Hydrophobicity refers to a molecule (hydrophobe) physical property mutually exclusive with water.Hydrophobic molecule is partial to nonpolar, and therefore can be dissolved in neutral and non-polar solution (as organic solution).The wettability of the surface of solids can be weighed with contact angle.While judging in addition the hydrophobic effect on a surface, also should consider its dynamic process, generally with roll angle, weigh.
Summary of the invention
What the present invention proposed is a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper, its objective is and uses corrugated paper as raw material, passes through Chemical Pretreatment; In conjunction with Mechanical Method grind, the processing such as ultrasonic makes nano-cellulose; The nanofiber cellulose solution and the nano titanium oxide that prepare is compound, under the coupled action of silane coupler, take the vacuum filtration mode to prepare at normal temperatures super-hydrophobic nano paper.
Technical solution of the present invention: a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper, tool originally comprise following three steps: (1) Chemical Pretreatment; (2) mechanical treatment, make nano-cellulose as the processing such as grinding, ultrasonic; Nanofiber cellulose solution and the nano titanium oxide that (3) will prepare are compound, under the effect of silane coupler, take the vacuum filtration mode to prepare at normal temperatures super-hydrophobic nano paper.
Advantage of the present invention: the concentration of the present invention's preparation is that the nanometer paper intensity of 10% titanium dioxide can reach 63MPa, and hydrophobic effect is good.The present invention is simple and easy to do, and is simple to operate, and equipment investment is little, can carry out large-scale production.
Description of drawings
Fig. 1 is the process chart that corrugated paper is prepared into nanofiber.
The specific embodiment
A kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper is characterized in that the method comprises: (1) Chemical Pretreatment; (2) mechanical treatment makes nano-cellulose; (3) prepare super-hydrophobic nano paper.
The described corrugated paper that utilizes prepares nanofiber process, it is characterized in that described Chemical Pretreatment comprises, 1) take the 10g corrugated paper,, with smashing and filter with mixer after distilled water immersion 1h, be settled to 500ml; 2) taking mass concentration is 2% NaOH 10g, in the situation that 90 ℃ of temperature are processed 2 ~ 4 h, cooling under room temperature after; 3) wash with distilled water until neutral; 4) take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, in the situation that temperature is 75 ℃, process three times, each one hour, then cooling standing in room temperature; 5) wash with distilled water until neutral; Take mass concentration and be 2% potassium hydroxide 10g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, then cooling standing under room temperature; 6) wash until neutral with distilled water.Take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, processed one hour in the situation that temperature is 75 ℃, then the standing room temperature that is cooled to; 7) wash until neutral with distilled water.Take 1% potassium hydroxide 5g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, cooling rear with distilled water washing until neutral; 8) measuring mass concentration with graduated cylinder is 36% hydrochloric acid 14ml, in the situation that temperature is 80 ℃, processes 2 ~ 4 h, cooling rear with the distilled water washing until neutrality obtains corrugation paper pulp.
The described method of utilizing corrugated paper to prepare nanofiber, is characterized in that described mechanical treatment is 1) chemical treatment and be washed till neutral corrugation paper pulp 500ml of learning from else's experience; 2) grind 20 times each 40min on grinder; 3) ultrasonic processing, get 50ml with the solution that is settled to 500ml and be diluted to 250ml and carry out ultrasonic processing 40min, and power is 1000W, makes nano-cellulose.
A kind of described method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper, is characterized in that the described super-hydrophobic nano paper for preparing, and concrete steps comprise:
(1) with silane coupler grafted nano titanium oxide in the system of alcohol: 1) take titanium dioxide nanoparticle 5 grams, it is dissolved in the system of 108 ml ethanols and 3 ml deionized water magnetic agitation 5 ~ 10 minutes; 2) dripping 1.52 gram concentration is the ammonia spirit of 25wt% and the silane coupler of 1.8g, and mixed solution is strong stirring 1 hour at normal temperatures; 3) solution is centrifugal in the absolute ethyl alcohol system by distilled water or ammoniacal liquor, purifying from silane coupler; 4) repeat repeatedly purifying, centrifugal, until there is no silane coupler in ethanol system; 5), through air dry in 24 hours, obtain the titanium dioxide nanoparticle of graft modification.
(2) prepare the hydrophobic paper of nano titanium oxide: comprise 1) get the nanofiber cellulose solution of preparation, adding the titanium dioxide nanoparticle of difference amount after silane coupler modified to the nanofiber cellulose solution, is to carry out high speed machine under the speed of 30000 rev/mins to mix at rotating speed; 2) the nanofiber cellulose solution after processing is ultrasonic, makes it fully dissolve and stir; 3) adopt the vacuum filtration machine to carry out vacuum filtration, namely obtain the hydrophobic paper of nano titanium oxide, flatten with clean glass plate, and be positioned over dry 48h in 60 degrees centigrade of baking ovens, afterwards dried film is placed on valve bag and seals up for safekeeping.
Embodiment 1
Utilize corrugated paper to prepare nanofiber process to be: Chemical Pretreatment comprises, 1) take the 10g corrugated paper, and, with smashing and filter with mixer after distilled water immersion 1h, be settled to 500ml; 2) taking mass concentration is 2% NaOH 10g, in the situation that 90 ℃ of temperature are processed 2 ~ 4 h, cooling under room temperature after; 3) wash with distilled water until neutral; 4) take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, in the situation that temperature is 75 ℃, process three times, each one hour, then cooling standing in room temperature; 5) wash with distilled water until neutral; Take mass concentration and be 2% potassium hydroxide 10g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, then cooling standing under room temperature; 6) wash until neutral with distilled water.Take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, processed one hour in the situation that temperature is 75 ℃, then the standing room temperature that is cooled to; 7) wash until neutral with distilled water.Take 1% potassium hydroxide 5g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, cooling rear with distilled water washing until neutral; 8) measuring mass concentration with graduated cylinder is 36% hydrochloric acid 14ml, in the situation that temperature is 80 ℃, processes 2 ~ 4 h, cooling rear with the distilled water washing until neutrality obtains corrugation paper pulp.
The mechanical treatment that corrugated paper prepares in the method for nanofiber is: the chemical treatment and be washed till neutral corrugation paper pulp 500ml of 1) learning from else's experience; 2) grind 20 times each 40min on grinder; 3) ultrasonic processing, get 50ml with the solution that is settled to 500ml and be diluted to 250ml and carry out ultrasonic processing 40min, and power is 1000W, makes nano-cellulose.
The present embodiment corrugated paper is prepared into the handling process of nanofiber and sees Fig. 1.
Embodiment 2
Prepare the hydrophobic paper of nano titanium oxide: the nanofiber cellulose solution of 1) getting preparation, be that 10% titanium dioxide after silane coupler modified adds the nanofiber cellulose solution to concentration, carry out high speed machine mixing 20min transferring under the speed of 25000 rev/mins; 2) solution after processing is ultrasonic, makes it fully dissolve and stir; 3) solution for preparing adopts the vacuum filtration machine to carry out vacuum filtration, namely obtains the hydrophobic paper of nano titanium oxide, flattens with clean glass plate, and is positioned over dry 48h in 60 ℃ of baking ovens, afterwards dried film is placed on valve bag and seals up for safekeeping.
Embodiment 3
Prepare the hydrophobic paper of nano titanium oxide: 1) getting the nanofiber cellulose solution of preparation, is that 20% titanium dioxide after silane coupler modified adds the nanofiber cellulose solution to concentration, carries out high speed machine under the speed of 30000 rev/mins and mixes transferring to; 2) solution after processing is ultrasonic, makes it fully dissolve and stir; 3) solution for preparing adopts the vacuum filtration machine to carry out vacuum filtration, namely obtains the hydrophobic paper of nano titanium oxide, flattens with clean glass plate, and is positioned over dry 48h in 60 ℃ of baking ovens, afterwards dried film is placed on valve bag and seals up for safekeeping.
Embodiment 4
Hydrophobicity test: adding concentration in nanofiber solution is 10% nano titanium oxide, the hydrophobicity on test nanometer paper surface.First comparatively smooth film is cut into the specimen of specification 4 * 4cm, drips a deionized water with small-sized syringe on sample, take pictures simultaneously, record and with contact angle instrument, measure contact angle.
Embodiment 5
Hydrophobicity test: adding concentration in nanofiber solution is 20% nano titanium oxide, the hydrophobicity on test nanometer paper surface.First comparatively smooth film is cut into the specimen of specification 4 * 4cm, drips a deionized water with small-sized syringe on sample, take pictures simultaneously, record and with contact angle instrument, measure contact angle.
Embodiment 6
Light transmittance: titanium dioxide concentration is the light transmittance of the 10% cellulose nano thin-film that makes after processing, and in visible wavelengths scope (400-800nm), the wavelength of light transmittance commonly used is chosen the 600nm place as benchmark.The light transmittance that pure nano-cellulose film records at the 600nm place is 80%, and after adding titanium dioxide in cellulose solution, titanium dioxide concentration is that 10% nano-cellulose film light transmittance is 65%.
Embodiment 7
Tensile property: pure nano-cellulose film TENSILE STRENGTH and elastic modelling quantity are respectively 74.16MPa and 2.17GPa; Titanium dioxide concentration is that 10% nano-cellulose film TENSILE STRENGTH and elastic modelling quantity are respectively 63.18MPa and 3.53GPa, and titanium dioxide concentration is that 20% nano-cellulose film TENSILE STRENGTH and elastic modelling quantity are respectively 50.48MPa, 2.63GPa,
The above-mentioned specific embodiment is exemplary, is in order can better to understand content of the present invention, to should not be understood as limiting the scope of the invention, so long as the improvement of doing according to technical solution of the present invention all falls into protection scope of the present invention.
Claims (4)
1. a method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper, is characterized in that the method comprises: (1) Chemical Pretreatment; (2) mechanical treatment makes nano-cellulose; (3) prepare super-hydrophobic nano paper.
2. a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper according to claim 1, it is characterized in that described Chemical Pretreatment comprises, 1) take the 10g corrugated paper,, with smashing and filter with mixer after distilled water immersion 1h, be settled to 500ml; 2) taking mass concentration is 2% NaOH 10g, in the situation that 90 ℃ of temperature are processed 2 ~ 4 h, cooling under room temperature after; 3) wash with distilled water until neutral; 4) take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, in the situation that temperature is 75 ℃, process three times, each one hour, then cooling standing in room temperature; 5) wash with distilled water until neutral; Take mass concentration and be 2% potassium hydroxide 10g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, then cooling standing under room temperature; 6) wash with distilled water until neutral; Take the sodium chlorite of 4.5g and measure the glacial acetic acid of 4ml, processed one hour in the situation that temperature is 75 ℃, then the standing room temperature that is cooled to; 7) wash with distilled water until neutral; Take 1% potassium hydroxide 5g, in the situation that temperature is 90 ℃, process 2 ~ 4 h, cooling rear with distilled water washing until neutral; 8) measuring mass concentration with graduated cylinder is 36% hydrochloric acid 14ml, in the situation that temperature is 80 ℃, processes 2 ~ 4 h, cooling rear with the distilled water washing until neutrality obtains corrugation paper pulp.
3. a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper according to claim 1, is characterized in that described mechanical treatment is the chemical treatment and be washed till neutral corrugation paper pulp 500ml of learning from else's experience; 2) grind 20 times each 40min on grinder; 3) ultrasonic processing, get 50ml with the solution that is settled to 500ml and be diluted to 250ml and carry out ultrasonic processing 40min, and power is 1000W, makes nano-cellulose.
4. a kind of method of utilizing corrugated paper/nano titanium oxide to prepare nano-sized hydrophobic paper according to claim 1, is characterized in that the described super-hydrophobic nano paper for preparing, and concrete steps comprise:
(1) with silane coupler grafted nano titanium oxide in the system of alcohol: 1) take titanium dioxide nanoparticle 5g, it is dissolved in the system of 108ml alcohol and 3ml deionized water magnetic agitation 5 ~ 10min; 2) dripping 1.52g concentration is the ammonia spirit of 25wt% and the silane coupler of 1.8g, and mixed solution is strong stirring 1 h at normal temperatures; 3) solution is centrifugal in the absolute ethyl alcohol system by distilled water or ammoniacal liquor, purifying from silane coupler; 4) repeat repeatedly purifying, centrifugal, until there is no silane coupler in ethanol system; 5), through 24 h air dries, obtain the titanium dioxide nanoparticle of graft modification;
(2) prepare the hydrophobic paper of nano titanium oxide: comprise 1) get the nanofiber cellulose solution of preparation, adding the titanium dioxide nanoparticle of difference amount after silane coupler modified to the nanofiber cellulose solution, is to carry out high speed machine under the speed of 30000 r/min to mix at rotating speed; 2) the nanofiber cellulose solution after processing is ultrasonic, makes it fully dissolve and stir; 3) adopt the vacuum filtration machine to carry out vacuum filtration, namely obtain the hydrophobic paper of nano titanium oxide, flatten with clean glass plate, and be positioned over dry 48h in 60 ℃ of baking ovens, afterwards dried film is placed on valve bag and seals up for safekeeping.
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| CN106317466A (en) * | 2016-08-19 | 2017-01-11 | 南京林业大学 | Method for preparing lithium battery diaphragm by compounding nano-cellulose and nano-silicon dioxide |
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| CN109162149A (en) * | 2018-07-18 | 2019-01-08 | 六安市星星包装股份有限公司 | A kind of production method of the super-hydrophobic compound corrugated case based on nano-titanium dioxide |
| CN111856227A (en) * | 2020-08-04 | 2020-10-30 | 江西理工大学 | Method for improving thermal aging resistance of converter transformer oil paper insulation and testing method |
| CN113976156A (en) * | 2021-10-19 | 2022-01-28 | 中南林业科技大学 | Preparation method of photocatalytic composite material with different wettability |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN111856227A (en) * | 2020-08-04 | 2020-10-30 | 江西理工大学 | Method for improving thermal aging resistance of converter transformer oil paper insulation and testing method |
| CN113976156A (en) * | 2021-10-19 | 2022-01-28 | 中南林业科技大学 | Preparation method of photocatalytic composite material with different wettability |
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Denomination of invention: A method for preparing nano hydrophobic paper using corrugated paper / nano titanium dioxide Effective date of registration: 20211215 Granted publication date: 20150603 Pledgee: Linshang Bank Co.,Ltd. Tancheng sub branch Pledgor: LINYI LIHUA PAPER INDUSTRY CO.,LTD. Registration number: Y2021980015127 |