CN109880345A - The poly-dopamine microballoon toughening polyurethane elastic composite and preparation method thereof of gamma ray resistant irradiation - Google Patents
The poly-dopamine microballoon toughening polyurethane elastic composite and preparation method thereof of gamma ray resistant irradiation Download PDFInfo
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Abstract
The invention discloses a kind of poly-dopamine microballoon toughening polyurethane elastic composites and preparation method thereof of gamma ray resistant irradiation, first prepare nanoscale poly-dopamine microballoon, microballoon after freeze-drying is uniformly dispersed in DMF equal solvent using cell pulverization Ultrasound Instrument, polyurethane elastomer is added；And it is dispersed in polyurethane matrix based on functional groups such as poly-dopamine microballoon catechol rich in, amino, mixed solution is poured into mold, solvent volatilizees to form poly-dopamine/polyurethane elastic composite material.The mass content of poly-dopamine microballoon is 1%~10% in composite material, and the partial size of poly-dopamine microballoon is 100~500nm.The poly-dopamine microballoon being dispersed in polyurethane not only acts as the effect of activeness and quietness, and effectively improves the anti-gamma-ray irradiation performance of material to the acquisition performance of free radical based on itself.
Description
Technical field
The present invention relates to field of polymer composite material, more particularly it relates to which a kind of irradiation of gamma ray resistant is poly-
Dopamine microballoon toughening polyurethane elastic composite and preparation method thereof.
Background technique
High molecular material is widely used in biomedicine, food packaging, health-oriented products and some special irradiation at present
Environment space.In such applications, always it is related to some ionizing radiations such as gamma-ray irradiation.And polymer is in gamma-ray irradiation
After can generate free radicals and ion.These free radicals can further cause or participate in degradation chemical reaction, as chain rupture, crosslinking,
Unsaturation reaction, causes the performance of material to be remarkably decreased.Degradation based on Induced By Irradiation strand is mainly radical reaction machine
Reason, therefore many researchers capture the free radical that irradiation generates by addition radical scavenger, prevent or reduce free radical
It is further to cause or participate in degradation reaction, so as to improve the radiation-resistant property of polymer.Wu Guozhang et al. utilizes oxidation
The free radical capture function of graphene effectively improves polyacrylic radiation-resistant property.M.J.Martinez-Morlanes is by carbon
Nanotube is added in polyethylene, confirms the free radical generated after its addition significantly lower than not by characterizations such as electron paramagnetic resonance
The polyethylene of addition effectively improves the radiation-resistant property of polyethylene.Although two-dimensional materials such as graphene oxide etc. are proved
With the good radiation-resistant property for improving polymer, but since difficulties in dispersion, poor compatibility are difficult equal in the polymer for itself
Even dispersion；Especially there are certain bio-toxicities in terms of some, therefore find some new free radical captures
Agent has certain meaning come the radiation-resistant property for improving polymer.
Summary of the invention
Easy preparation, good biocompatibility, the easily poly-dopamine microballoon that disperses are added in polyurethane material by the present invention, have
Effect utilizes the free radical capture function of poly-dopamine microballoon, enhances the radiation-resistant property of polyurethane.Based on poly-dopamine microballoon
Biocompatibility and its surface group abundant, microballoon is uniformly dispersed in the polymer and no biotoxicity, enhances to it
While the effect of toughening, the multifunctionality of compound polyurethane material is effectively improved, expands its application range.
In order to reach above-mentioned technical effect, the present invention takes following technical scheme:
A kind of poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, by the poly- DOPA of nanoscale
Amine microballoon, which is dispersed in polyurethane elastomer, to be formed, and the good composite material of compatibility, poly-dopamine in composite material are formed
The mass content of microballoon is 1%~10%, and the partial size of poly-dopamine microballoon is 100~500nm.
The present invention also provides the poly-dopamine microballoon toughening polyurethane elastomer composites for preparing above-mentioned gamma ray resistant irradiation
The method of material first prepares nanoscale poly-dopamine microballoon, and the microballoon after freeze-drying is uniform using cell pulverization Ultrasound Instrument
Be dispersed in DMF equal solvent, be added polyurethane elastomer；And it is based on poly-dopamine microballoon catechol rich in, ammonia
Ji Deng functional group is dispersed in it in polyurethane matrix, and mixed solution is poured into mold, solvent volatilize to be formed poly-dopamine/
Polyurethane elastic composite material.The poly-dopamine microballoon being dispersed in polyurethane not only acts as the effect of activeness and quietness, and
And the anti-radiation performance for the material that the acquisition performance of free radical is effectively improved based on itself.The preparation method specifically includes
Following steps:
Step A prepares poly-dopamine microballoon
The buffer solution of meta-alkalescence is configured, addition ethyl alcohol, dopamine particle stir evenly, and make dopamine in slight alkali environment
Lower carry out polymerization reaction forms poly-dopamine microballoon, and it is micro- that nanometer poly-dopamine is obtained by multiple eccentric cleaning, after freeze-drying
Ball；
Step B prepares composite material
In organic solvent by the dispersion of poly-dopamine microballoon, PU particle is added, stirring and dissolving after mixing, is polymerize
Object solution, is poured into mold and forms a film, and after film forming, is put into room temperature in vacuum drying oven and vacuumizes the remaining organic solvent of removal,
Obtain composite material.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step A
Used in dopamine particle be dopamine salt granulates, the PU particle that step B is used is poly- [4,4'- di-2-ethylhexylphosphine oxide (isocyanic acids
Phenyl ester)-alt-1,4- butanediol/bis- (propylene glycol)/polycaprolactone.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step A
In slight alkali environment refer to reaction solution pH be 8~10；The mass concentration of dopamine is 0.1%~1% in reaction solution；It is described
The reaction time of polymerization reaction be 5~for 24 hours.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step A
There is the feature of fluffy dispersion by the poly-dopamine microballoon of freeze-drying, in favor of dispersing in a polymer solution.
It is described poly- in the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation
The partial size of dopamine microballoon is 100~500nm.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step B
Poly-dopamine microballoon is dispersed using cell pulverization Ultrasound Instrument in organic solvent, to prevent poly-dopamine microballoon from reuniting.
It is described multiple in the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation
The mass content of poly-dopamine microballoon is 1%~10% in condensation material.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step B
The organic solvent is selected from least one of N,N-dimethylformamide, ethyl acetate.
In the method for preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, step B
Used in mold be Teflon mould, but mold is not limited to polytetrafluoroethylene (PTFE).The pumpdown time of the vacuum drying oven
For 24~48h, it is therefore intended that remove extra solvent.Mold shape is different, can obtain composite material of different shapes.
Poly-dopamine is a kind of natural black pigment at present, nontoxic to have very high biocompatibility, and since its surface contains
There are a large amount of tea polyphenols and amino group, can be attracted wide public concern in the polymer such as dispersion very high in polyurethane.Through
It confirms, poly-dopamine has the function of significant free radical capture due to its special structure.And dopamine is put into the water of alkalinity
Polymer reaction will be caused in solution, without reaction conditions such as other initiators or heating, preparation process is simple, is easy to get.
Therefore it is added in biological polyurethane while enhance its radiation-resistant property, also having improves its biocompatibility
Function.Furthermore nanoscale poly-dopamine microballoon can effectively increase the breaking strength and fracture deformation of polyurethane elastomer used
Rate.
The present invention is based on the free radical mechanism of Induced By Irradiation polymer molecule chain reaction, has free radical by addition
The poly-dopamine microballoon of capturing function further causes preventing or reduce free radical or participates in reaction, so as to improve polyurethane
Radiation-resistant property.This method can design the composite material of different shape, cavernous structure and different function according to actual needs.
This composite material can effectively improve the radiation-resistant property of material.In addition, poly-dopamine microballoon can be effective as nanofiller
The effect that activeness and quietness is played to elastic polyurethane matrix.
Compared with prior art, the present invention at least has the advantages that
(1) the method for the present invention forms composite material into polyurethane by adding poly-dopamine microballoon, effectively improves
While the gamma ray resistant irradiation behaviour of polyurethane, play the role of activeness and quietness to its mechanical property.It is demonstrate,proved by later experiments
It is modified in fact still to remain the mechanical mechanics almost the same with non-irradiated elastic polyurethane matrix after 200kGy irradiates
Energy.And its mechanical property degradation of the polyurethane elastomer of filler is not added under same irradiation dose.
(2) the method for the present invention preparation process is simple, experiment condition is mild, safety is good, does not need to be modified filler,
Added material poly-dopamine is a kind of natural black pigment, good biocompatibility, and due to its surface there are also a large amount of tea polyphenols and
Amino group has dispersibility well in the polymer, can further expand the application range of compound polyurethane material.
Detailed description of the invention
Fig. 1 is the poly-dopamine microballoon shape appearance figure after freeze-drying.
Fig. 2 is different poly-dopamine content (0wt%:a, b；1wt%:c, d) compound polyurethane material pass through 0kGy
(a, c), the surface sweeping Electronic Speculum cross-sectional view after 200kGy (b, d) gamma-ray irradiation.
Fig. 3 is the stress-strain diagram of the compound polyurethane material of different poly-dopamine contents under 0kGy effect.
Fig. 4 is the stress-strain diagram of the compound polyurethane material of different poly-dopamine contents under 200kGy effect.
Fig. 5 is the breaking strength figure before and after the compound polyurethane material 200kGy irradiation dose of different poly-dopamine contents.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Embodiment 1
(1) 360mL H is measured2O, 72mL ethyl alcohol weigh 0.892g 2- amino -2- (methylol) -1,3-PD and enter to burn
In cup, after 1000rpm stirs 20min, 540mg Dopamine hydrochloride is added, pH value is about 8~10, for 24 hours with 300rpm stirring, from
The heart is simultaneously cleaned three times with deionized water, and freeze-drying obtains poly-dopamine microballoon.Its partial size is in 200nm or so.
(2) the poly-dopamine microballoon 0.1g prepared in step (1) is weighed, is added in 100g n,N-Dimethylformamide,
Ultrasonic disperse is carried out using cell pulverization Ultrasound Instrument (II D of SCIENTZ-), ultrasonic time 20min, the time, super 2s stopped 1s.Ultrasound is complete
9.9g PU particle is added in Cheng Hou, after 400rpm rate mechanical stirring 48h, stops stirring, after a period of stabilisation, imports poly-
It forms a film in tetrafluoroethene (PTFE) mold.After film forming, it is put into vacuum drying oven room temperature 30h, remaining organic solvent is removed, obtains
Obtaining the poly-dopamine microballoon toughening polyurethane elastic composite that gamma ray resistant irradiates, (abbreviation poly-dopamine/polyurethane is compound
Material).
Embodiment 2
Method is with embodiment 1, the difference is that weighing the poly-dopamine microballoon 0.25g prepared in step (1) in step (2).
Embodiment 3
Method is with embodiment 1, the difference is that weighing the poly-dopamine microballoon 0.5g prepared in step (1) in step (2).
Embodiment 4
Method is with embodiment 1, the difference is that weighing the poly-dopamine microballoon 0.75g prepared in step (1) in step (2).
Embodiment 5
Method is with embodiment 1, the difference is that weighing the poly-dopamine microballoon 1g prepared in step (1) in step (2).
There is poly-dopamine/compound polyurethane material performance of radiation-resistant property to survey 1~5 gained of above-described embodiment
Examination:
1. irradiation behaviour
Irradiation bomb is60Co gamma-ray irradiation (Chinese gongwu researcher nuclear physics research institute provides).Sample is in air
Middle receiving irradiates accumulated dose 50kGy~200kGy, radiation dose rate 90Gy/min.
2. the performance test analysis such as pattern, mechanics after predose
Stress-strain test is in RSA G2, test rate 0.83mm/s.Using FE-SEM, ZEISSUltra 55 is right
Pattern after polymer predose is characterized.
The present invention scans electricity using the poly-dopamine microballoon after the freeze-drying prepared in the method and step (1) of embodiment 1
Mirror figure.Poly-dopamine microballoon is circle as can be seen from Figure 1, is uniformly dispersed.
The compound polyurethane material and polyurethane material containing 1wt% poly-dopamine microballoon prepared in embodiment illustrated in fig. 21
Expect the cross-sectional scans electron microscope of the material after 200kGy irradiation dose.As can be seen from Figure, polyurethane material is passing through
After the irradiation of 200kGy irradiation dose, surface occurs damaged；And after adding poly-dopamine formation composite material, under same radiation parameter
Substantially variation is not seen in surface.
Fig. 3 is the stress-strain diagram of the compound polyurethane material of different poly-dopamine mass contents under 0kGy effect.Through scheming
In find out, with the increase of filler poly-dopamine microspheres amount, under the same conditions, the tear type variability of composite material and fracture
Intensity enhances, and illustrates that nanofiller plays the role of activeness and quietness.
Fig. 4 is the stress-strain diagram of the compound polyurethane material of 200kGy difference poly-dopamine mass content.With irradiation
The breaking strain decrease speed of the increase of dosage, polyurethane elastomer is very fast, and the compound polyurethane material containing poly-dopamine
Preferable tear type variability is still kept under the conditions ofs same irradiation temperature, irradiation dose etc..
Fig. 5 is the intensity map after the compound polyurethane material 200kGy predose of different poly-dopamine contents.It can from figure
To find out, addition poly-dopamine microballoon can effectively improve the breaking strength decline degree of polymer, have certain anti-spoke
According to ability.The compound polyurethane material breaking strength of 5wt% poly-dopamine content after 200kGy is irradiated still is slightly above
Non-irradiated polyurethane elastomer.And pure polyurethane elastomer its breaking strength sharp fall.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, however, it is to be understood that ability
Field technique personnel can be designed that a lot of other modification and implementations, these modifications and implementations will fall in the application public affairs
Within the scope and spirit opened.It more specifically, can be to the group of theme combination layout in range disclosed in the present application
A variety of variations and modifications are carried out at component and/or layout.In addition to variations and improvements to the component parts and or layout,
To those skilled in the art, other purposes also will be apparent.
Claims (10)
1. a kind of poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation, it is characterised in that nanoscale
Poly-dopamine microballoon is dispersed in polyurethane elastomer, in composite material the mass content of poly-dopamine microballoon be 1%~
10%, the partial size of poly-dopamine microballoon is 10~500nm.
2. preparing the poly-dopamine microballoon toughening polyurethane elastic composite of gamma ray resistant irradiation described in claim 1
Method, it is characterised in that the following steps are included:
Step A prepares poly-dopamine microballoon
Configure the buffer solution of meta-alkalescence, ethyl alcohol, dopamine particle be added and stirs evenly, make dopamine under slight alkali environment into
Row polymerization reaction forms poly-dopamine microballoon, and by multiple eccentric cleaning, nanometer poly-dopamine microballoon is obtained after freeze-drying；
Step B prepares composite material
By poly-dopamine microballoon dispersion in organic solvent, be added PU particle, stirring and dissolving after mixing, pour into mold at
Film after film forming, is put into room temperature in vacuum drying oven and vacuumizes the remaining organic solvent of removal, obtain composite material.
3. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that dopamine particle used in step A is dopamine salt granulates, the PU particle that step B is used
For poly- [4,4'- di-2-ethylhexylphosphine oxides (phenyl isocyanate)-alt-1,4- butanediol/bis- (propylene glycol)/polycaprolactone.
4. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that in step A, slight alkali environment refers to that the pH of reaction solution is 8~10；The matter of dopamine in reaction solution
Measuring concentration is 0.1%~1%；The reaction time of the polymerization reaction be 5~for 24 hours.
5. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that step A has the feature of fluffy dispersion by the poly-dopamine microballoon of freeze-drying.
6. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that the partial size of the poly-dopamine microballoon is 100~500nm.
7. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that in step B, poly-dopamine microballoon is dispersed in organic solvent using cell pulverization Ultrasound Instrument,
Prevent poly-dopamine microballoon from reuniting.
8. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that in the composite material, the mass content of poly-dopamine microballoon is 1%~10%.
9. the poly-dopamine microballoon toughening polyurethane elastomer composite material according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that in step B, the organic solvent in n,N-Dimethylformamide, ethyl acetate at least
It is a kind of.
10. the poly-dopamine microballoon toughening polyurethane elastomer composite according to claim 2 for preparing gamma ray resistant irradiation
The method of material, it is characterised in that mold used in step B is Teflon mould, when vacuumizing of the vacuum drying oven
Between be 24~48h.
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| CN111410887A (en) * | 2020-05-11 | 2020-07-14 | 郑明光 | Super-hydrophobic nano SiO2 modified epoxy acrylic resin coating and preparation method thereof |
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| CN113248853A (en) * | 2021-07-15 | 2021-08-13 | 北京石墨烯技术研究院有限公司 | Sealing element and method for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113248853A (en) * | 2021-07-15 | 2021-08-13 | 北京石墨烯技术研究院有限公司 | Sealing element and method for producing same |
| CN113248853B (en) * | 2021-07-15 | 2021-09-21 | 北京石墨烯技术研究院有限公司 | Sealing element and method for producing same |
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