CN110240723A - Ultraviolet high shielding fiber element film of one kind and the preparation method and application thereof - Google Patents
Ultraviolet high shielding fiber element film of one kind and the preparation method and application thereof Download PDFInfo
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- CN110240723A CN110240723A CN201910645351.0A CN201910645351A CN110240723A CN 110240723 A CN110240723 A CN 110240723A CN 201910645351 A CN201910645351 A CN 201910645351A CN 110240723 A CN110240723 A CN 110240723A
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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
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- C08J5/18—Manufacture of films or sheets
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention belongs to functional living being degradative membranes, disclose ultraviolet high shielding fiber element film of one kind and the preparation method and application thereof.Cerium salt and halloysite nanotubes are uniformly mixed by the method specially (1) in a solvent obtains mixed solution, then ammonium hydroxide is added and hexa carries out heating reaction, it is after reaction that products therefrom is dry, then after heat treatment, obtain galapectite-cerium oxide nano hybrid；(2) galapectite-cerium oxide nano hybrid and cellulose are distributed in water respectively, then two kinds of dispersion liquids of gained is uniformly mixed and obtain mixed dispersion liquid, then resulting mixed dispersion liquid is dried to obtain ultraviolet high shielding fiber element film.This cellulose membrane have it is ultraviolet shielded it is high-efficient, thermal stability is excellent, mechanical strength is good, flexibility is good, transparency is higher, asepsis environment-protecting, many merits such as biodegradable, and preparation is simple for the cellulose membrane, low raw-material cost can be widely used for the fields such as ultraviolet protection.
Description
Technical field
The invention belongs to functional living being degradative membrane fields, and in particular to the ultraviolet high shielding fiber element film of one kind and its preparation
Method and application.
Background technique
Currently, the ultraviolet light for reaching earth's surface is remarkably reinforced with the continuous destruction of ozone layer, to human health, material
Stability all causes serious harm, therefore, needs to develop a kind of product for capableing of high-efficiency shielding ultraviolet light.Cerium oxide is one
Nontoxic, the environmentally friendly inorganic rare earth ultraviolet light screener of kind, has obtained extensively in fields such as composite material, building coating, daily chemical products
General application.However, cerium oxide nano particle surface can be higher, easily reunite, seriously affected cerium oxide nano particle
Ultraviolet shielded efficiency.
In recent years, the application of loaded catalyst causes the extensive concern of scientific circles and industry, is inspired by this, studies
Persons load to organic additive, noble metal, metal oxide etc. on nano grade inorganic carrier, are prepared for a series of functionality and receive
Rice hybrid particle, significantly improve the performances such as anti-aging, Industrial Catalysis, conduction, photocatalysis (1.Zhong B, Shi Q, Jia Z,
et al.Preparation of silica-supported 2-mercaptobenzimidazole and its
antioxidative behavior in styrene-butadiene rubber[J].Polymer Degradation and
Stability,2014,110:260-267；2.Xue B,Chen P,Hong Q,et al.Growth of Pd,Pt,Ag and
Au nanoparticles on carbon nanotubes[J].Journal of Materials Chemistry,2001,
11(9):2378-2381；3.Liu B,Zeng H C.Carbon Nanotubes Supported Mesoporous
Mesocrystals of Anatase TiO2[J].Chemistry of Materials,2008,20(8):2711-2718；
4.CN107308964A a kind of preparation method of galapectite load indium phosphate catalyst；5.CN101999411A halloysite nanotubes
Load silver-colored simple substance type antibacterial agent and preparation method thereof；6.CN106732566A a kind of carbon nanotube loaded metal ruthenium nano particle is urged
The preparation method of agent；7.CN107425185A the preparation method of a kind of carbon nanotube loaded carbonization molybdenum material and its in lithium sulphur
Application in cell positive material).However in ultraviolet shielded field, there is not yet improving the report of uv-shielding capacity using this method
Road.
Summary of the invention
The defects of in order to overcome current cerium oxide nano particle easy to reunite, ultraviolet shielded low efficiency, primary mesh of the invention
Be to provide and a kind of there is ultraviolet high shielding fiber element film.
Another object of the present invention is to provide a kind of preparation method of above-mentioned ultraviolet high shielding fiber element film；It is of the present invention
The cellulose membrane of ultraviolet high shielding utilize cellulose and galapectite-cerium oxide nano hybrid preparation.Wherein galapectite-
Cerium oxide nano hybrid is that cerium oxide nano particle is carried on to the obtained one kind in halloysite nanotubes surface in situ is novel
Nano hybrid, the hybrid can effectively improve the agglomeration of cerium oxide nano particle.
Still a further object of the present invention is to provide application of the above-mentioned ultraviolet high shielding fiber element film in ultraviolet protection field.
A kind of preparation method of ultraviolet high shielding fiber element film, includes the following steps:
(1) cerium salt and halloysite nanotubes are uniformly mixed in a solvent and obtain mixed solution, ammonium hydroxide and six is then added
Methenamine carries out heating reaction, after reaction that products therefrom is dry, then after heat treatment, obtains galapectite-oxidation
Cerium nano hybrid；
(2) galapectite-cerium oxide nano hybrid of step (1) preparation and cellulose are distributed in water respectively, then
Two kinds of dispersion liquids of gained are uniformly mixed and obtain mixed dispersion liquid, then resulting mixed dispersion liquid is dried to obtain ultraviolet height
Shielding fiber element film.
Preferably, cerium salt described in step (1) is at least one of cerous sulfate, cerous acetate, cerium chloride and cerous nitrate；
Preferably, solvent described in step (1) is the mixed solvent of organic solvent and water；Wherein water accounts for the total matter of mixed solvent
The 20-50% of amount；The organic solvent is preferably at least one of ethyl alcohol and methanol.
Preferably, the dosage of halloysite nanotubes described in step (1) is the 0.5-3% of solvent quality；
Preferably, the additional amount of cerium salt described in step (1) is the 50-200% of halloysite nanotubes quality；
Preferably, step (1) is described is uniformly mixed as ultrasonic 10-60min；
Preferably, the dosage of step (1) described ammonium hydroxide, which meets, is adjusted to 8-10 for the pH value of mixed solution；
Preferably, the dosage of hexa described in step (1) is 2-5 times of cerium salt quality；
Preferably, step (1) the heating reaction is to react 1-3 hours at 60-100 DEG C；
Preferably, step (1) is described further includes the steps that purifying products therefrom after reaction；
Preferably, step (1) heat treatment is to be heat-treated 1-3 hours at 400-480 DEG C.
Preferably, cellulose described in step (2) is cellulose nano-fibrous, nano micro crystal cellulose, fibrillation fiber
At least one of modified celluloses such as element, bacteria cellulose and carboxymethyl cellulose；
Preferably, galapectite-cerium oxide nano hybrid and cellulose gross mass in step (2) described mixed dispersion liquid
Concentration is 0.15wt.%-0.6wt.%, and wherein galapectite-cerium oxide nano hybrid additional amount is the 1- of cellulose quality
20%.
Preferably, step (2) is uniformly mixed as ultrasonic 10-60min；
Preferably, step (2) drying is 3-7 hours dry at 30-70 DEG C after filtering gained mixed dispersion liquid
Or it is directly that resulting mixed dispersion liquid is 8-24 hours dry at 30-70 DEG C.
A kind of ultraviolet high shielding fiber element film being prepared according to the above method.
Application of the above-mentioned ultraviolet high shielding fiber film in ultraviolet protection field.Especially in parasol, beach umbrella, glass
The fields such as glass fenestrated membrane, outdoor protective materials have good application.
In addition, the present invention prepares halloysite nanotubes-cerium oxide nano hybrid using ammonium hydroxide and hexa, instead
Short between seasonable, reaction condition is mild, and the ceria partial size on especially surface is more uniform, can be applied not only to cellulose membrane
In, all there is potential application prospect in the daily chemical products such as other polymers matrix, coating, suncream.
Ultraviolet high shielding fiber element film prepared by the present invention has the advantage that and special compared with traditional ultraviolet shielded film
Color:
1, efficiently: cellulose membrane prepared by the present invention is realized by the way that galapectite-cerium oxide nano hybrid is modified；Angstrom
Lip river stone nanotube-cerium oxide nano hybrid has unique nano hybridization structure, high-specific surface area, the cerium oxide nano on surface
The uniform particle sizes of particle, without serious agglomeration, so that the tunica fibrosa of preparation has high ultraviolet shielded efficiency；
2, multi-functional: in cellulose membrane prepared by the present invention, the galapectite with one-dimensional nano structure and high thermal stability
Nano-carrier can significantly improve the mechanical property and thermal stability of cellulose membrane simultaneously, thus prepared by the present invention is that one kind is more
Functional cellulose membrane；
3, environmentally friendly: in primary raw material used in the present invention, halloysite nanotubes and cellulose are natural material；And
The film of preparation is biodegradable, can efficiently reduce white pollution；
4, easily industrialization: cellulose membrane moulding process of the invention is simple and easy, without complicated process equipment；Nanometer is miscellaneous
The reaction time of compound is short, reaction is mild；Required material source approach is extensive, low in cost, is easier to realize large-scale application.
Detailed description of the invention
Fig. 1 is that the present invention prepares galapectite-cerium oxide nano hybrid schematic illustration.
Fig. 2 is galapectite-cerium oxide nano hybrid SEM figure prepared by embodiment 1.
Fig. 3 is galapectite-cerium oxide nano hybrid TEM figure prepared by embodiment 1.
Fig. 4 is the digital pictures of cellulose membrane prepared by embodiment 2.
Fig. 5 is the digital pictures of cellulose membrane prepared by comparative example 2.
Specific embodiment
The present invention is described in further detail with attached drawing combined with specific embodiments below, but embodiments of the present invention
It is without being limited thereto, for not specifically specified technological parameter, it can refer to routine techniques progress.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
In the mixed solvent by 1g halloysite nanotubes and 1g cerous acetate ultrasonic disperse to 80g water and 80g ethyl alcohol, ultrasound
After 20min, addition ammonium hydroxide adjusts pH value to 9, adds the hexa of 3.2g, reacts 2 hours at 75 DEG C；Then second is used
It is 12 hours dry in 60 DEG C of vacuum drying oven after alcohol and water distinguishes centrifuge washing three times；Again by obtained product at 450 DEG C
Calcining heat treatment 2 hours, obtains halloysite nanotubes-cerium oxide nano hybrid.By halloysite nanotubes-cerium oxide of preparation
Nano hybrid and it is cellulose nano-fibrous be distributed in deionized water respectively, by two dispersion liquids mix after, gained mixing dispersion
Total mass concentration is 0.2wt.% in liquid, and wherein galapectite-cerium oxide nano hybrid additive amount is cellulose quality
5%.Then filter cake is dried 5 hours celluloses modified to get hybrid by vacuum filtration by ultrasonic 30min at 60 DEG C
Film.
Fig. 2 is 1 halloysite nanotubes of gained embodiment-cerium oxide nano hybrid SEM figure；Fig. 3 is 1 gained of embodiment
Halloysite nanotubes-cerium oxide nano hybrid TEM figure.It can be seen from the figure that cerium oxide nano particle uniformly combines
On the surface of halloysite nanotubes.Ultraviolet shielded efficiency difference of the prepared cellulose hybrid membrane within the scope of UVA, UVB, UVC
Reach 49%, 58% and 87%.Thermogravimetic analysis (TGA) the result shows that, hybrid is modified, the weightless peak temperature ratio of the maximum of composite membrane
Pure cellulose membrane improves 26.3 DEG C, and thermal stability significantly improves.
Embodiment 2
In the mixed solvent by 3g halloysite nanotubes and 1.5g cerous nitrate ultrasonic disperse to 40g water and 60g ethyl alcohol, ultrasound
60min, addition ammonium hydroxide adjust pH value to 10, then add the hexa of 3g, react 1 hour at 100 DEG C；Use ethyl alcohol
It is 6 hours dry in 80 DEG C of vacuum drying oven after distinguishing centrifuge washing three times with water；Obtained product is calcined at 400 DEG C
Heat treatment 3 hours, obtains halloysite nanotubes-cerium oxide nano hybrid.By the cellulose of the hybrid of preparation and fibrillation
It is distributed in deionized water respectively, after two dispersion liquids are mixed, total mass concentration is in gained mixed dispersion liquid
0.15wt.%, wherein galapectite-cerium oxide nano hybrid additive amount is the 1% of cellulose quality.Ultrasonic 10min, passes through
Filter cake is dried 3 hours cellulose membranes modified to get hybrid by vacuum filtration at 70 DEG C.It as a comparison, will be after ultrasound
Mixed dispersion liquid is directly poured into mold, can obtain cellulose membrane within dry 8 hours at 70 DEG C.To shorten drying time, improve fine
The interface cohesion for tieing up plain film and hybrid, is preferably filtered by vacuum the mode combined with vacuum drying.
Fig. 4 is the digital pictures of the cellulose membrane prepared, it can be seen from the figure that under modified composite membrane visible light
The transparency is still very high.
Embodiment 3
In the mixed solvent by 0.5g halloysite nanotubes and 1g cerous sulfate ultrasonic disperse to 20g water and 80g ethyl alcohol, ultrasound
10min, addition ammonium hydroxide adjust pH value to 8, the hexa of 5g are then added, reacts 3 hours at 60 DEG C；With ethyl alcohol and
It is 18 hours dry in 50 DEG C of vacuum drying oven after water distinguishes centrifuge washing three times；Obtained product is calcined to heat at 480 DEG C
Processing 1 hour, obtains halloysite nanotubes-cerium oxide nano hybrid.By the hybrid of preparation and nano micro crystal cellulose point
It not being distributed in deionized water, after two dispersion liquids are mixed, total mass concentration is 0.6wt.% in gained mixed dispersion liquid,
Middle galapectite-cerium oxide nano hybrid additive amount is the 20% of cellulose quality.Ultrasonic 60min, by vacuum filtration, so
Filter cake is dried to 7 hours cellulose membranes modified to get hybrid at 30 DEG C afterwards.Prepared cellulose membrane it is ultraviolet shielded
Efficiency is 95% or more.
Embodiment 4
In the mixed solvent by 1g halloysite nanotubes and 1g cerous acetate ultrasonic disperse to 80g water and 80g ethyl alcohol, ultrasound
30min, addition ammonium hydroxide adjust pH value to 9, then add the hexa of 3.2g, react 2 hours at 75 DEG C；Use ethyl alcohol
It is 12 hours dry in 60 DEG C of vacuum drying oven after distinguishing centrifuge washing three times with water；Obtained product is calcined at 450 DEG C
Heat treatment 2 hours, obtains halloysite nanotubes-cerium oxide nano hybrid.By the hybrid of preparation and carboxymethyl cellulose point
It not being distributed in deionized water, after two dispersion liquids are mixed, total mass concentration is 0.35wt.% in gained mixed dispersion liquid,
Wherein galapectite-cerium oxide nano hybrid additive amount is the 10% of cellulose quality.Ultrasonic 30min, then directly pours into
In mold, and the dry 18 hours cellulose membranes modified to get hybrid at 50 DEG C, the ultraviolet screen of prepared cellulose membrane
It covers efficiency and reaches 83%.
Embodiment 5
In the mixed solvent by 1g halloysite nanotubes and 0.5g cerous acetate ultrasonic disperse to 50g water and 50g ethyl alcohol, ultrasound
40min, addition ammonium hydroxide adjust pH value to 10, the hexa of 2g are added, 70℃Lower reaction 1.5 hours；With second alcohol and water
It is 6 hours dry in 80 DEG C of vacuum drying oven after distinguishing centrifuge washing three times；By obtained product 450℃Lower calcining heat treatment
2 hours, obtain halloysite nanotubes-cerium oxide nano hybrid.The hybrid of preparation and bacteria cellulose are distributed to respectively
In deionized water, after two dispersion liquids are mixed, total mass concentration is 0.35wt.% in gained mixed dispersion liquid, wherein angstrom Lip river
Stone-cerium oxide nano hybrid additive amount is the 10% of cellulose quality.Ultrasonic 30min, directly pours into mold, at 30 DEG C
The lower drying 24 hours cellulose membranes modified to get hybrid, the ultraviolet shielded efficiency of prepared cellulose membrane is more than 80%.
Embodiment 6
In the mixed solvent by 1g halloysite nanotubes and 1g cerous nitrate ultrasonic disperse to 40g water and 60g ethyl alcohol, ultrasound
Then 60min adds ammonium hydroxide and adjusts pH value to 8, and adds the hexa of 3g, react 3 hours at 65 DEG C；Use ethyl alcohol
It is 6 hours dry in 80 DEG C of vacuum drying oven after distinguishing centrifuge washing three times with water；Obtained product is calcined at 480 DEG C
Heat treatment 1 hour, obtains halloysite nanotubes-cerium oxide nano hybrid.By the hybrid of preparation and cellulose nano-fibrous
It is distributed in deionized water respectively, after two dispersion liquids are mixed, total mass concentration is in gained mixed dispersion liquid
0.26wt.%, wherein galapectite-cerium oxide nano hybrid additive amount is the 7% of cellulose quality.Ultrasonic 20min, passes through
Filter cake is dried 5 hours cellulose membranes modified to get hybrid by vacuum filtration at 60 DEG C, prepared cellulose membrane
Ultraviolet shielded efficiency is 73%.
Comparative example 1
As a comparison, it prepared by the cerium oxide of equivalent and halloysite nanotubes substitution galapectite-cerium oxide nano hybrid
Tunica fibrosa, other preparation conditions and additive amount are consistent with embodiment 6.
The ultraviolet shielded efficiency of prepared cellulose membrane is only 68%, and ultraviolet shielded significant effect is lower than galapectite-oxygen
Change the cellulose membrane of cerium nano hybrid preparation, and the transmitance of the cellulose membrane of the comparative example 1 preparation under visible light is lower than
The modified cellulose membrane of galapectite-cerium oxide hybrid, the transparency of composite membrane are severely impacted.
Comparative example 2
As a comparison, it prepared by the cerium oxide of equivalent and halloysite nanotubes substitution galapectite-cerium oxide nano hybrid
Tunica fibrosa, other preparation conditions and additive amount are consistent with embodiment 2.
Fig. 5 is the digital pictures of cellulose membrane prepared by embodiment 2, it can be seen from the figure that compared with Example 2, adding
After the cerium oxide and halloysite nanotubes that add equivalent, it is seen that serious reduce occurs in the transparency under light.
The above embodiment of the present invention is not to this hair merely to the specific case for clearly demonstrating the present invention and lifting
The restriction of bright embodiment.For those of ordinary skill in the art, it can also be made on the basis of the above description
Its various forms of change.All technology and methods according to the present invention are substantially to the above embodiments any simply to repair
Change, equivalent variations and improvement, should be included within the scope of protection of the claims of the present invention.
Claims (8)
1. a kind of preparation method of ultraviolet high shielding fiber element film, which comprises the steps of:
(1) cerium salt and halloysite nanotubes are uniformly mixed in a solvent and obtain mixed solution, ammonium hydroxide and six methylenes are then added
Urotropine carries out heating reaction, after reaction that products therefrom is dry, then after heat treatment, obtains galapectite-cerium oxide and receive
Rice hybrid；
(2) galapectite-cerium oxide nano hybrid of step (1) preparation and cellulose are distributed in water respectively, then by institute
Two kinds of dispersion liquids are uniformly mixed and obtain mixed dispersion liquid, then resulting mixed dispersion liquid is dried to obtain ultraviolet high shield
Cellulose membrane.
2. the preparation method of ultraviolet high shielding fiber element film according to claim 1, it is characterised in that:
Cerium salt described in step (1) is one of cerous sulfate, cerous acetate, cerium chloride, cerous nitrate；
Solvent described in step (1) is the mixed solvent of organic solvent and water.
3. the preparation method of ultraviolet high shielding fiber element film according to claim 1, it is characterised in that:
The dosage of halloysite nanotubes described in step (1) is the 0.5-3% of solvent quality；
The additional amount of cerium salt described in step (1) is the 50-200% of halloysite nanotubes quality；
The dosage of ammonium hydroxide described in step (1), which meets, is adjusted to 8-10 for the pH value of mixed solution；
The dosage of hexa described in step (1) is 2-5 times of cerium salt quality.
4. the preparation method of ultraviolet high shielding fiber element film according to claim 1, it is characterised in that:
Step (1) the heating reaction is to react 1-3 hours at 60-100 DEG C；
Step (1) heat treatment is to be heat-treated 1-3 hours at 400-480 DEG C.
5. the preparation method of ultraviolet high shielding fiber element film according to claim 1, it is characterised in that:
Cellulose described in step (2) is cellulose nano-fibrous, nano micro crystal cellulose, fento cellulose, bacterial fibers
At least one of element and carboxymethyl cellulose.
6. the preparation method of ultraviolet high shielding fiber element film according to claim 1, it is characterised in that:
The total mass concentration of galapectite-cerium oxide nano hybrid and cellulose is in step (2) described mixed dispersion liquid
0.15wt.%-0.6wt.%, wherein galapectite-cerium oxide nano hybrid additional amount is the 1- of cellulose quality
20%.
7. a kind of any one ultraviolet high shielding fiber element film according to claim 1~6.
8. application of the ultraviolet high shielding fiber element film in ultraviolet protection field according to claim 7.
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| CN112175243A (en) * | 2020-09-21 | 2021-01-05 | 桂林理工大学 | High-performance cellulose acetate composite material and preparation method thereof |
| CN112239564A (en) * | 2020-09-21 | 2021-01-19 | 桂林理工大学 | Cellulose acetate nano composite material with ultraviolet shielding function and preparation method thereof |
| CN113788989A (en) * | 2021-09-13 | 2021-12-14 | 桂林理工大学 | Starch-based nano composite material with ultraviolet shielding function and preparation method thereof |
| CN116509756A (en) * | 2023-05-18 | 2023-08-01 | 广东暨纳新材料科技有限公司 | Composite sun-screening emulsion based on cerium oxide clay and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175243A (en) * | 2020-09-21 | 2021-01-05 | 桂林理工大学 | High-performance cellulose acetate composite material and preparation method thereof |
| CN112239564A (en) * | 2020-09-21 | 2021-01-19 | 桂林理工大学 | Cellulose acetate nano composite material with ultraviolet shielding function and preparation method thereof |
| CN113788989A (en) * | 2021-09-13 | 2021-12-14 | 桂林理工大学 | Starch-based nano composite material with ultraviolet shielding function and preparation method thereof |
| CN113788989B (en) * | 2021-09-13 | 2023-05-30 | 桂林理工大学 | Starch-based nanocomposite with ultraviolet shielding function and preparation method thereof |
| CN116509756A (en) * | 2023-05-18 | 2023-08-01 | 广东暨纳新材料科技有限公司 | Composite sun-screening emulsion based on cerium oxide clay and preparation method thereof |
| CN116509756B (en) * | 2023-05-18 | 2024-01-23 | 广东暨纳新材料科技有限公司 | Composite sun-screening emulsion based on cerium oxide clay and preparation method thereof |
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| CN110240723B (en) | 2022-05-17 |
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