CN107540857A - A kind of anti-flaming nano film and preparation method and application - Google Patents
A kind of anti-flaming nano film and preparation method and application Download PDFInfo
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- CN107540857A CN107540857A CN201710756014.XA CN201710756014A CN107540857A CN 107540857 A CN107540857 A CN 107540857A CN 201710756014 A CN201710756014 A CN 201710756014A CN 107540857 A CN107540857 A CN 107540857A
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Abstract
The invention belongs to field of nanometer material technology, discloses a kind of anti-flaming nano film and preparation method and application.A kind of preparation method of described anti-flaming nano film is：Ball-milling treatment is carried out after hydroxyapatite is dried, ultrasonic cell-break obtains nanometer hydroxyapatite emulsion after processing a period of time；Blend solution is made according to certain adding proportion in nano-cellulose and nanometer hydroxyapatite, film forming obtains anti-flaming nano film under the conditions of constant temperature and humidity.A kind of anti-flaming nano film has good anti-flammability, and nano-cellulose and nanometer hydroxyapatite have good biocompatibility, can apply in fields such as fire proofing, flexible electronic device, biomaterials.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of anti-flaming nano film and preparation method and application.
Background technology
China is both that the big producer of chemical fibre consumes big country again, but fire resistance fibre accounts for chemical fibre total amount at present
Ratio it is also very low, although the research of China's Prospect for Flame Retardant Fiber Materials originates in last century middle nineteen sixties, fire-retardant skill
Art development is slower, so the flame-retardant modified technology of fiber is one of direction of current research.
Cellulose is that a kind of polysaccharide most wide, that content is most are distributed in nature, is D-Glucose with β-Isosorbide-5-Nitrae glycosidic bond
The existing high-molecular compound of composition.But there is many defects, such as intensity in native cellulose in physical aspect and chemical property
Low, pyrolysis poor performance, not corrosion-resistant etc..Nano-cellulose refers to that fiber has a dimension to reach 1-100nm on three dimensions
Size be nano-cellulose.Nano-cellulose has unique physics, chemical property, as size is small, specific surface area is big and
Crystallinity height etc., there is huge potential using value in papermaking, food, cosmetics, electronic device and biomedical sector.
Hydroxyapatite is the host inorganic constituent of vertebrate skeletal and tooth, has excellent biocompatibility
And bioactivity, it can apply to the fields such as biomaterial, ion exchange, catalysis and insoluble drug release.Nanometer hydroxyapatite is
Size is less than 100nm hydroxyapatite crystal.
The report on nanometer hydroxyapatite is the application on it in biomedical sector mostly at present, there is no on
Nano-cellulose and nanometer hydroxyapatite prepare the report of fire proofing.
The content of the invention
The shortcomings that in order to overcome prior art and deficiency, primary and foremost purpose of the invention are to provide a kind of new fire-retardant receive
Rice membrane material.
Another object of the present invention is to provide the preparation method of above-mentioned anti-flaming nano film.
It is yet a further object of the present invention to provide the application of above-mentioned anti-flaming nano film.Anti-flaming nano prepared by the present invention
Film, it can be applied in fields such as flexible electronic device, biomaterial and medical materials, expand nano-cellulose and hydroxy-apatite
The application of stone.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of anti-flaming nano film, is comprised the steps of：
(1) ball-milling treatment is carried out after hydroxyapatite is dried, ultrasonic cell-break is received after processing a period of time
Rice hydroxyapatite emulsion；
(2) 0~16% adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose quality, will receive
Rice hydroxyapatite emulsion, which is added in nano-cellulose solution, is made blend solution, and film forming is hindered under the conditions of constant temperature and humidity
Fire nanometer film.
Preferably, the temperature of step (1) described drying is 80~110 DEG C, and the time is 5~24h；12~72h of ball-milling treatment.
It is furthermore preferred that drying temperature is 105 DEG C, time 12h；Ball-milling treatment 48h.
Preferably, ultrasonic cell-break condition is described in step (1)：Power is 800w, power output 10~40%,
The broken time is 10~60min.
Preferably, step (1) described nano-cellulose is using straw pulp of rice and wheat as raw material, after base extraction, is used
The method oxidized fibre of TEMPO oxidations, then be made after carrying out secondary high-pressure homogenization.Received using prepared by TEMPO oxidizing process
Rice cellulose surface also contains substantial amounts of carboxyl, preferably can coexist and combine with nanometer hydroxyapatite, is formed firm
Chemical bond.
The alkali lye is the NaOH solution that mass concentration is 15%.
The TEMPO oxidizing conditions are：NaBr, TEMPO and NaClO addition difference in every gram of over dry rice wheat straw fiber
For 0.1~0.2g, 0.01~0.03g and (0.5~0.75) g, rice wheat straw fiber concentration is 0.5~2wt%, the reaction time 1
~3h, pH=10.0~10.3, rotating speed are 100~500r/min；NaBr, TEMPO in preferably every gram of over dry rice wheat straw fiber
Addition with NaClO is 0.15g, 0.015g and (0.5~0.75) g, and rice wheat straw fiber concentration is 2wt%, and the reaction time is
1.5h, pH=10.0~10.3, rotating speed 500r/min.
The secondary high-pressure homogenization is：First handled 2 times under the conditions of pressure is 10000psi, then in pressure
Handled 5 times under the conditions of 25000psi.
Preferably, the quality adding proportion of nanometer hydroxyapatite described in step (2) is over dry nano-cellulose quality
4~16%.
Preferably, constant temperature and humidity condition is described in step (2)：Temperature is 30~80 DEG C, and humidity is 40~90%, the time
For 24~72h.
A kind of anti-flaming nano film has good anti-flammability, and nano-cellulose and nano hydroxyapatite made from the above method
Lime stone has good biocompatibility, can apply in fields such as fire proofing, biomedical material, flexible electronic devices.
The flame-retarding characteristic of hydroxyapatite is utilized in the present invention, by hydroxyapatite sized nanostructures, is added to Nanowire
Tie up in plain thin-film material, there is catalysis characteristics due to hydroxyapatite, the formation speed and neat coal amout of layer of charcoal may be improved,
Therefore the fire resistance of composite membrane is improved.In addition, nanometer hydroxyapatite is attached to the surface of fiber, the hole of film is filled and led up, is made
Nano-cellulose film becomes finer and close and smooth, the circulation of oxygen in film has been separated in burning, so as to reach fire-retardant effect
Fruit, you can play flame retardant effect.
Compared with prior art, the present invention has advantages below and beneficial effect：
Anti-flaming nano film of the present invention, will have flame-retarding characteristic hydroxyapatite sized nanostructures after, be added to and receive
In rice cellophane, there is catalysis characteristics due to hydroxyapatite, the formation speed and neat coal amout of layer of charcoal may be improved,
Therefore the fire resistance of composite membrane is improved.Nanometer hydroxyapatite is attached in the surface and space of fiber, so that cellulose
Film becomes fine and close and smooth, the inside that oxygen enters film is effectively separated in burning, so as to reach fire-retardant effect.This method exists
The application of hydroxyapatite and nano-cellulose is have also been enlarged while a kind of novel flame-retardant membrane material is provided.
Brief description of the drawings
Fig. 1 is a kind of preparation process schematic diagram of anti-flaming nano film.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of anti-flaming nano film, its preparation method are as follows：
(1) after handling straw pulp of rice and wheat with 15wt% NaOH solution, in the rice wheat straw fiber after every gram of over dry alkali process
NaBr, TEMPO and NaClO addition are respectively 0.15g, 0.015g and 0.6g, and it is 2wt%, reaction time 1.5h that slurry is dense,
PH=10.0~10.3, rotating speed 500r/min.It is first 10000psi in pressure with high pressure homogenizer after TEMPO oxidation processes
Under the conditions of handle 2 times, then handled 5 times under the conditions of pressure 25000psi and obtain nano-cellulose.
(2) nano-cellulose is configured to solution, the film forming under the conditions of the constant temperature and humidity that temperature is 30 DEG C, humidity is 90%
Anti-flaming nano film is obtained after 48h.
The limited oxygen index of the nanometer film prepared by oxygen index measurer measure is 24.4%, belongs to combustible material.
Embodiment 2
A kind of anti-flaming nano film, its preparation method are as follows：
(1) after handling straw pulp of rice and wheat with 15wt% NaOH solution, in the rice wheat straw fiber after every gram of over dry alkali process
NaBr, TEMPO and NaClO addition are respectively 0.15g, 0.015g and 0.6g, and it is 2wt%, reaction time 1.5h that slurry is dense,
PH=10.0~10.3, rotating speed 500r/min.It is first 10000psi in pressure with high pressure homogenizer after TEMPO oxidation processes
Under the conditions of handle 2 times, then handled 5 times under the conditions of pressure 25000psi and obtain nano-cellulose.
(2) hydroxyapatite is dried into 12h at 110 DEG C to take out, after then carrying out ball-milling treatment 72h, is with power
800w ultrasonic cell-break machine, power output are adjusted to 30%, and processing 20min obtains nanometer hydroxyapatite emulsion.
(3) the quality adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose 4%, by nano-hydroxy
Apatite emulsion is added in nano-cellulose solution and blend solution is made, permanent in the constant temperature that temperature is 40 DEG C, humidity is 95%
Anti-flaming nano film is obtained under the conditions of wet after film forming 72h.
The limited oxygen index of the nanometer film prepared by oxygen index measurer measure is 28.7%, belongs to combustible material.
Embodiment 3
(1) after handling straw pulp of rice and wheat with 15wt% NaOH solution, in the rice wheat straw fiber after every gram of over dry alkali process
NaBr, TEMPO and NaClO addition are respectively 0.15g, 0.015g and 0.6g, and it is 2wt%, reaction time 1.5h that slurry is dense,
PH=10.0~10.3, rotating speed 500r/min.It is first 10000psi in pressure with high pressure homogenizer after TEMPO oxidation processes
Under the conditions of handle 2 times, then handled 5 times under the conditions of pressure 25000psi and obtain nano-cellulose.
(2) hydroxyapatite is dried into 24h at 100 DEG C to take out, after then carrying out ball-milling treatment 48h, is with power
800w ultrasonic cell-break machine, power output are adjusted to 40%, and processing 10min obtains nanometer hydroxyapatite emulsion.
(3) the quality adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose 8%, by nano-hydroxy
Apatite emulsion is added in nano-cellulose solution and blend solution is made, permanent in the constant temperature that temperature is 80 DEG C, humidity is 40%
Anti-flaming nano film is obtained under the conditions of wet after film forming 24h.
The limited oxygen index of the nanometer film prepared by oxygen index measurer measure is 30.2%, belongs to combustible material.
Embodiment 4
(1) after handling straw pulp of rice and wheat with 15wt% NaOH solution, in the rice wheat straw fiber after every gram of over dry alkali process
NaBr, TEMPO and NaClO addition are respectively 0.15g, 0.015g and 0.6g, and it is 2wt%, reaction time 1.5h that slurry is dense,
PH=10.0~10.3, rotating speed 500r/min.It is first 10000psi in pressure with high pressure homogenizer after TEMPO oxidation processes
Under the conditions of handle 2 times, then handled 5 times under the conditions of pressure 25000psi and obtain nano-cellulose.
(2) hydroxyapatite is dried into 18h at 90 DEG C to take out, is 800w with power after then carrying out ball-milling treatment 36h
Ultrasonic cell-break machine, power output is adjusted to 20%, and processing 30min obtains nanometer hydroxyapatite emulsion.
(3) the quality adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose 12%, by nanometer hydroxyl
Base apatite emulsion, which is added in nano-cellulose solution, is made blend solution, in the constant temperature that temperature is 60 DEG C, humidity is 90%
Anti-flaming nano film is obtained under the conditions of constant humidity after film forming 36h.
The limited oxygen index of the nanometer film prepared by oxygen index measurer measure is 31.1%, belongs to combustible material.
Embodiment 5
(1) after handling straw pulp of rice and wheat with 15wt% NaOH solution, in the rice wheat straw fiber after every gram of over dry alkali process
NaBr, TEMPO and NaClO addition are respectively 0.15g, 0.015g and 0.6g, and it is 2wt%, reaction time 1.5h that slurry is dense,
PH=10.0~10.3, rotating speed 500r/min.It is first 10000psi in pressure with high pressure homogenizer after TEMPO oxidation processes
Under the conditions of handle 2 times, then handled 5 times under the conditions of pressure 25000psi and obtain nano-cellulose.
(2) hydroxyapatite is dried into 10h at 105 DEG C to take out, after then carrying out ball-milling treatment 48h, is with power
800w ultrasonic cell-break machine, power output are adjusted to 20%, and processing 30min obtains nanometer hydroxyapatite emulsion.
(3) the quality adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose 16%, by nanometer hydroxyl
Base apatite emulsion, which is added in nano-cellulose solution, is made blend solution, in the constant temperature that temperature is 50 DEG C, humidity is 90%
Anti-flaming nano film is obtained under the conditions of constant humidity after film forming 48h.
The limited oxygen index of the nanometer film prepared by oxygen index measurer measure is 31.3%, belongs to combustible material.
The test of the anti-flaming nano film oxygen barrier properties of embodiment 6
The fire resistance for the anti-flaming nano film that embodiment 1~5 is prepared detects, and tester is JF-3 type oxygen
Indexer, method of testing are as shown in table 1 with reference to GB/T 2406-93, test result.
The limited oxygen index test result of the anti-flaming nano film of table 1.
| Nanometer hydroxyapatite addition (wt%) | Limited oxygen index (%) |
| 0 | 24.4 |
| 4 | 28.7 |
| 8 | 30.2 |
| 12 | 31.1 |
| 16 | 31.3 |
From table 1, the limited oxygen index value of the film of non-plus nano hydroxyapatite is 24%, belongs to combustible material；With
The increase of nanometer hydroxyapatite addition, the limited oxygen index value of film increases, and illustrates the addition of nanometer hydroxyapatite
Serve fire-retardant effect.When nanometer hydroxyapatite addition is 12wt%, oxygen index value 31.1%, belonging to can fuel wood
Material；Continue the addition mass ratio of increasing nanometer hydroxyapatite, the limited oxygen index of membrane material is not significantly improved, now
The anti-flammability of film reaches flame-retardant standard.The adding proportion of the optimal nanometer hydroxyapatite of the present invention is 12%.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of anti-flaming nano film, it is characterised in that comprise the steps of：
(1) ball-milling treatment is carried out after hydroxyapatite is dried, ultrasonic cell-break obtains a nanometer hydroxyl after processing a period of time
Base apatite emulsion；
(2) 0~16% adding proportion according to nanometer hydroxyapatite relative to over dry nano-cellulose quality, by nanometer hydroxyl
Base apatite emulsion, which is added in nano-cellulose solution, is made blend solution, and film forming obtains fire-retardant receive under the conditions of constant temperature and humidity
Rice film.
A kind of 2. preparation method of anti-flaming nano film according to claim 1, it is characterised in that step (1) described nanometer
Cellulose is using straw pulp of rice and wheat as raw material, after base extraction, using the method oxidized fibre of TEMPO oxidations, then carries out two
It is made after sub-high pressure homogenization.
A kind of 3. preparation method of anti-flaming nano film according to claim 1, it is characterised in that step (1) described drying
Temperature be 80~110 DEG C, the time is 5~24h；12~72h of ball-milling treatment.
4. the preparation method of a kind of anti-flaming nano film according to claim 1, it is characterised in that surpass described in step (1)
Sound wave clasmatosis condition is：Power is 800w, and power output 10~40%, it is 10~60min to crush the time.
5. the preparation method of a kind of anti-flaming nano film according to claim 1, it is characterised in that step is received described in (2)
The quality adding proportion of rice hydroxyapatite is the 4~16% of over dry nano-cellulose quality.
6. the preparation method of a kind of anti-flaming nano film according to claim 1, it is characterised in that permanent described in step (2)
Constant temperature and humidity condition is：Temperature is 30~80 DEG C, and humidity is 40~90%, and the time is 24~72h.
7. a kind of anti-flaming nano film, it is characterised in that it is as a kind of anti-flaming nano film described in any one of claim 1 to 6
Preparation method is made.
8. the anti-flaming nano film described in claim 7 is in fire proofing, biomedical material and flexible electronic device field
Using.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109400963A (en) * | 2018-10-15 | 2019-03-01 | 桂林理工大学 | A kind of preparation method of graphene-based flame-proof heat-resistant sisal cellulose film |
| CN109679208A (en) * | 2018-12-14 | 2019-04-26 | 金旸（厦门）新材料科技有限公司 | A kind of environment-friendly high-efficiency anti-flaming polypropylene composite and preparation method thereof |
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