CN105860509A - Modified carbon nanotube-toughened TPU film and preparation method thereof - Google Patents
Modified carbon nanotube-toughened TPU film and preparation method thereof Download PDFInfo
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- CN105860509A CN105860509A CN201610405233.9A CN201610405233A CN105860509A CN 105860509 A CN105860509 A CN 105860509A CN 201610405233 A CN201610405233 A CN 201610405233A CN 105860509 A CN105860509 A CN 105860509A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
A modified carbon nanotube-toughened TPU film is prepared from, by weight, 100 parts of polyether type TPU particles, 2-10 parts of modified carbon nanotubes and 0.1-5 parts of an antioxidant, wherein polymethyl methacrylate-modified single-wall carbon nanotubes are adopted as the modified carbon nanotubes. According to the TPU film, the flexibility is significantly improved.
Description
Technical field
The present invention relates to a kind of TPU film and preparation method thereof, particularly relate to a kind of CNT toughening modifying
TPU film and preparation method thereof.
Background technology
TPU (Thermoplastic polyurethanes) entitled Polyurethane Thermoplastic Elastomer rubber, mainly
Be divided into have polyester-type and polyether-type point.Its hardness range width (60HA-85HD), wear-resisting, oil resistant, transparent,
Good springiness, is used widely in fields such as article of everyday use, sports goods, toy, ornament materials.
TPU film is on the basis of TPU particulate material, through the special process such as calendering, curtain coating, blown film, coating
The thin film made.TPU (thermoplastic polyurethane) is increasingly subject to people because of its superior performance and environmental protection concept
Welcome.At present, the place of every use PVC, TPU all can become the succedaneum of PVC.But TPU
The advantage being had, PVC is the most too far behind to catch up.TPU not only has the high-tension of brilliance, high-tensile strength, tough
With ageing-resistant characteristic, and it is kind of ripe environment-friendly materials.At present, TPU is widely used in: footwear
Material, ready-made clothes, inflatable toys, waterborne and sports equipment under water, medical device, body-building apparatus, automobile seat
Seat material, umbrella, leather trunk, suitcase etc..
CNT, due to its exclusive structure and peculiar Wuli-Shili-Renli system approach, has just become since coming out
One of worldwide study hotspot.The good characteristic of CNT includes | anisotropy, high machinery are strong
Degree and elastic, excellent heat-conductivity conducting etc..How to be applied in TPU material by CNT is also this neck
One of direction of territory research.
The system of the thermoplastic polyurethane film of a kind of loading multi-wall carbon nanotubes is disclosed such as CN 101724981A
Preparation Method, first carries out early stage process to CNT, it is thus achieved that carboxylic carbon nano-tube, then by correspondence TPU
Ultrasonic disperse in the solvent of corresponding TPU mass 2-2.2 times of carboxylic carbon nano-tube addition of quality 0.1%-5%
0.5-2 hour, add TPU and continue the CNTs/TPU composite solution that ultrasonic agitation 1-2 hour acquisition is homogeneous,
And obtain membranoid substance by the method for electrostatic spinning.The fracture strength of this invention gained thin film, Young's modulus are aobvious
Write and strengthen, but elongation at break is but remarkably decreased.
Summary of the invention
For solving the problems referred to above, it is thin that an object of the present invention is to provide a kind of CNT toughening modifying TPU
Film.The TPU film toughness that the present invention provides dramatically increases.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of CNT toughening modifying TPU film, includes following component by weight:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 2-10 part
Antioxidant 0.1-5 part
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified.
Described modified carbon nano-tube can be such as 3,6 parts, 8 parts, 9 parts etc..
Described antioxidant can be such as 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1.0 parts, 1.5 parts, 2.0 parts,
2.5 parts, 3.1 parts, 3.6 parts, 4.0 parts, 4.4 parts, 4.8 parts etc..
The combination using said components proportioning and specific modified carbon nano-tube can improve prepared thin film significantly
Toughness.Expected effect is can be only achieved, not above-mentioned in the component only selected in the present invention and content range
Component and content range in then do not reach intended technique effect.Visible, the said components of the present invention and containing
Amount cooperates, and jointly acts on, and achieves unforeseeable technique effect, it is seen that the performance of embodiment part
Test.
As preferably, the CNT toughening modifying TPU film of the present invention, include following one-tenth by weight
Point:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 4-8 part
Antioxidant 0.5-3 part
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified.
As preferably, the CNT toughening modifying TPU film of the present invention, described antioxidant is polyphenol antioxygen
Agent and the combination of phosphite antioxidant.
Preferably, described polyphenol antioxidant is antioxidant 1010 and/or antioxidant 1076.
Preferably, described phosphite antioxidant is irgasfos 168 and/or 618.
Preferably, described polyphenol antioxidant is 1:0.2-5 with the mol ratio of phosphite antioxidant, for example,
1:0.4,1:0.7,1:1.1,1:1.5,1:2,1:2.6,1:3.3,1:3.8,1:4.2,1:4.7 etc., under this ratio
Polyphenol antioxidant and phosphite combination can obtain the antioxidant effect of excellence, preferably 1:1-3.
Preferably, the SWCN of described polymethyl methacrylate modification is prepared via a method which,
Comprise the steps:
(1) SWCN and polymethyl methacrylate are dissolved in dichloromethane, then indifferent gas
The lower reaction of body protection；
(2) reacted mixture is cooled to room temperature, and then with dchloromethane, the solution after dilution is used
Micro-pore-film filtration；
(3) filtrate after filtering is drying to obtain the SWCN that polymethyl methacrylate is modified.
Preferably, step (1) described SWCN with the mol ratio of polymethyl methacrylate is
1:0.05-0.5。
Preferably, the temperature of described reaction is 90-110 DEG C, and the time of reaction is 24-72h, preferably 36-50
h。
Preferably, the aperture of step (2) described microporous membrane is 0.2-0.4 μm, preferably polyvinylidene fluoride
Microporous membrane.
Preferably, the described dry temperature of step (3) is 90-110 DEG C, and the time being dried is 5-10h.
The thin film of the present invention adds the modified CNT of said method can be greatly increased the toughness of prepared thin film.
" including " of the present invention, it is intended that it is in addition to described component, it is also possible to include other components, these its
He gives the characteristic that described TPU film is different at component.In addition, " including " of the present invention, also may be used
With replace with enclosed " being " or " by ... composition ".
It is thin that an object of the present invention also resides in a kind of CNT toughening modifying TPU of the present invention of offer
The preparation method of film, comprises the steps:
(1) will mix after raw material drying；
(2) mixed material melt blending is obtained composite master batch；
(3) masterbatch is carried out blown film, calendering or casting film-forming processing, obtains described TPU film.
As preferably, in the preparation method of the present invention, it is dried under vacuo at 50-70 DEG C described in step (1),
For example, 53 DEG C, 57 DEG C, 60 DEG C, 64 DEG C, carry out under 68 DEG C etc. more than 2h, for example, 2.2h, 2.6h,
3.3h, 3.9h, 4.5h, 5.7h, 7.5h etc., preferably 3-6h.
Preferably, it is blended in described in high-speed mixer and carries out.
Preferably, the time of described mixing is more than 1min, for example, 2min, 2.5min, 3.4min, 4
Min, 4.5min etc., preferably 3-5min.
Preferably, during described mixing, mixer rotating speed is more than 20000r/min, preferably 30000-50000
r/min。
As preferably, in the preparation method of the present invention, described in step (2), the temperature of melt blending is
150-230 DEG C, for example, 155 DEG C, 160 DEG C, 163 DEG C, 168 DEG C, 172 DEG C, 177 DEG C, 185 DEG C, 190 DEG C,
195 DEG C, 201 DEG C, 207 DEG C, 215 DEG C, 226 DEG C etc., the time is 0.5-5h, for example, 0.8h, 1.5h,
3h, 3.6h, 4.5h etc., preferably 1-2h.
The present invention adds the SWCN of modification in TPU granule, the TPU film product making to prepare
Toughness changes significantly.The situation that the tensile strength of the elastic polyurethane body thin film that the present invention prepares is suitable with comparative example
Under, elongation at break dramatically increases, it is seen that the present invention prepares the pliability of thin film and is obviously enhanced.
Detailed description of the invention
For the present invention is better described, it is simple to understand technical scheme, the typical case of the present invention but non-limit
The embodiment of property processed is as follows:
Embodiment 1
A kind of CNT toughening modifying TPU film, includes following component by weight:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 10 parts
0.5 part of antioxidant
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified；
Described antioxidant is antioxidant 1010 and phosphite antioxidant 618 mol ratio is the combination of 1:5；
And be prepared by the following method:
(1) raw material is dried under vacuo at 60 DEG C mixing after more than 3h；
(2) by mixed material in high-speed mixer at 170 DEG C, rotating speed is that 40000r/min is melted altogether
Mixed 3h obtains composite master batch；
(3) masterbatch is carried out blown film processing, obtain described TPU film.
Embodiment 2
A kind of CNT toughening modifying TPU film, includes following component by weight:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 2 parts
5 parts of antioxidant
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified；
Described antioxidant is antioxidant 1076 and phosphite antioxidant 168 mol ratio is the combination of 1:0.2；
And be prepared by the following method:
(1) raw material is dried under vacuo at 70 DEG C mixing after more than 5h；
(2) by mixed material in high-speed mixer at 150 DEG C, rotating speed is that 50000r/min is melted altogether
Mixed 0.5h obtains composite master batch；
(3) masterbatch is carried out casting film-forming processing, obtain described TPU film.
Embodiment 3
A kind of CNT toughening modifying TPU film, includes following component by weight:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 5 parts
0.1 part of antioxidant
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified；
Described antioxidant be polyphenol antioxidant 1010 be the combination of 1:1 with phosphite antioxidant 168 mol ratio；
And be prepared by the following method:
(1) mix after raw material being dried 2h under vacuo at 50 DEG C；
(2) by mixed material in high-speed mixer at 230 DEG C, rotating speed is that 20000r/min is melted altogether
Mixed 2.5h obtains composite master batch；
(3) carry out masterbatch rolling film forming processing, obtain described TPU film.
Comparative example 1
Embodiment 2 in CN 101724981A.
Comparative example 2
Difference from Example 1 is: antioxidant is that antioxidant 1010 rubs with phosphite antioxidant 618
You are than the combination for 1:0.1.
Comparative example 3
Difference from Example 2 is: CNT is SWCN；Antioxidant is phosphite ester
Antioxidant 618.
Comparative example 4
Difference from Example 3 is: polyether-type TPU granule 100 parts, modified carbon nano-tube 1 part,
8 parts of antioxidant.
Performance test
The film product that embodiment 1-3 and comparative example prepare is carried out physical property measurement, the results are shown in Table 1.
Table 1
As known from Table 1, the tensile strength of the elastic polyurethane body thin film of embodiment of the present invention 1-3 and comparative example phase
In the case of when, elongation at break dramatically increases, and illustrates that the present invention prepares the pliability of thin film and is obviously enhanced.
The concrete ratio of the material that the antioxidant of comparative example 2 uses not within the scope of this application, comparative example 3
Then use CNT be SWCN be not that the application limits, the carbon modified of comparative example 4 is received
Mitron, antioxidant amount not within the scope of this application.But, result but shows, the product of the present invention
In the case of tensile strength is suitable with comparative example, elongation at break dramatically increases, it is seen that only limit in the present invention
Preferable effect could be obtained in fixed component and corresponding content range.
Applicant states, person of ordinary skill in the field is on the basis of above-described embodiment, by above-mentioned reality
Execute the concrete content point value of example component, combined with the technical scheme of Summary, thus produce
New numerical range, is also one of the record scope of the present invention, the application for making description simple and clear, no longer sieve
Arrange these numerical rangies.
Applicant states, the present invention illustrates the present invention by above-described embodiment, but the present invention does not limit to
In aforesaid operations step, i.e. do not mean that the present invention has to rely on aforesaid operations step and could implement.Affiliated skill
The technical staff in art field it will be clearly understood that any improvement in the present invention, to raw material selected by the present invention etc.
Effect is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within protection scope of the present invention and public affairs
Within the scope of opening.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned enforcement
Detail in mode, in the technology concept of the present invention, can enter technical scheme
The multiple simple variant of row, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention,
In the case of reconcilable, can be combined by any suitable means, in order to avoid unnecessary weight
Multiple, various possible compound modes are illustrated by the present invention the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is not
Running counter to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a CNT toughening modifying TPU film, includes following component by weight:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 2-10 part
Antioxidant 0.1-5 part
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified.
CNT toughening modifying TPU film the most according to claim 1, it is characterised in that by weight
Amount number includes following component:
Polyether-type TPU granule 100 parts
Modified carbon nano-tube 4-8 part
Antioxidant 0.5-3 part
Wherein, described modified carbon nano-tube is the SWCN that polymethyl methacrylate is modified.
CNT toughening modifying TPU film the most according to claim 1 and 2, it is characterised in that
Described antioxidant is the combination of polyphenol antioxidant and phosphite antioxidant；
Preferably, described polyphenol antioxidant is antioxidant 1010 and/or antioxidant 1076；
Preferably, described phosphite antioxidant is irgasfos 168 and/or 618；
Preferably, described polyphenol antioxidant is 1:0.2-5 with the mol ratio of phosphite antioxidant, is preferably
1:1-3。
4., according to the CNT toughening modifying TPU film described in any one of claim 1-3, its feature exists
In, the SWCN of described polymethyl methacrylate modification is prepared via a method which, including as follows
Step:
(1) SWCN and polymethyl methacrylate are dissolved in dichloromethane, then indifferent gas
The lower reaction of body protection；
(2) reacted mixture is cooled to room temperature, and then with dchloromethane, the solution after dilution is used
Micro-pore-film filtration；
(3) filtrate after filtering is drying to obtain the SWCN that polymethyl methacrylate is modified.
CNT toughening modifying TPU film the most according to claim 4, it is characterised in that step
(1) described SWCN is 1:0.05-0.5 with the mol ratio of polymethyl methacrylate；
Preferably, the temperature of described reaction is 90-110 DEG C, and the time of reaction is 24-72h, preferably 36-50
h。
6. according to the CNT toughening modifying TPU film described in claim 4 or 5, it is characterised in that
The aperture of step (2) described microporous membrane is 0.2-0.4 μm, preferably polyvinylidene fluoride microporous membrane；
Preferably, the described dry temperature of step (3) is 90-110 DEG C, and the time being dried is 5-10h.
7. the preparation method of the TPU film described in any one of claim 1-6, comprises the steps:
(1) will mix after raw material drying；
(2) mixed material melt blending is obtained composite master batch；
(3) masterbatch is carried out blown film, calendering or casting film-forming processing, obtains described TPU film.
Preparation method the most according to claim 7, it is characterised in that be dried described in step (1)
More than 2h, preferably 3-6h is carried out under vacuo at 50-70 DEG C.
9. according to the preparation method described in claim 7 or 8, it is characterised in that described in step (1)
It is blended in high-speed mixer and carries out；
Preferably, the time of described mixing is more than 1min, preferably 3-5min；
Preferably, during described mixing, mixer rotating speed is more than 20000r/min, preferably 30000-50000
r/min。
10. according to the preparation method described in any one of claim 7-9, it is characterised in that in step (2)
The temperature of described melt blending is 150-230 DEG C, and the time is 0.5-5h, preferably 1-2h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610405233.9A CN105860509A (en) | 2016-06-08 | 2016-06-08 | Modified carbon nanotube-toughened TPU film and preparation method thereof |
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| CN201610405233.9A CN105860509A (en) | 2016-06-08 | 2016-06-08 | Modified carbon nanotube-toughened TPU film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349333A (en) * | 2020-04-21 | 2020-06-30 | 东莞市雄林新材料科技股份有限公司 | TPU film for surfing kite and preparation method thereof |
| CN112961489A (en) * | 2021-02-05 | 2021-06-15 | 深圳鑫富艺科技股份有限公司 | High-ductility TPU film and preparation method thereof |
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| CN103386258A (en) * | 2013-06-29 | 2013-11-13 | 浙江工业大学 | Preparation method of polyamide composite nanofiltration membrane containing modified carbon nano tube |
| CN103694140A (en) * | 2013-12-02 | 2014-04-02 | 艾达索高新材料无锡有限公司 | Degradable isocyanate and application thereof |
| CN104177581A (en) * | 2013-05-27 | 2014-12-03 | 拜耳材料科技(中国)有限公司 | Polyurethane composition for polyurethane composite material |
| CN104987701A (en) * | 2015-07-22 | 2015-10-21 | 东莞市雄林新材料科技股份有限公司 | Electrostrictive TPU film and preparation method and application thereof |
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2016
- 2016-06-08 CN CN201610405233.9A patent/CN105860509A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177581A (en) * | 2013-05-27 | 2014-12-03 | 拜耳材料科技(中国)有限公司 | Polyurethane composition for polyurethane composite material |
| CN103386258A (en) * | 2013-06-29 | 2013-11-13 | 浙江工业大学 | Preparation method of polyamide composite nanofiltration membrane containing modified carbon nano tube |
| CN103694140A (en) * | 2013-12-02 | 2014-04-02 | 艾达索高新材料无锡有限公司 | Degradable isocyanate and application thereof |
| CN104987701A (en) * | 2015-07-22 | 2015-10-21 | 东莞市雄林新材料科技股份有限公司 | Electrostrictive TPU film and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349333A (en) * | 2020-04-21 | 2020-06-30 | 东莞市雄林新材料科技股份有限公司 | TPU film for surfing kite and preparation method thereof |
| CN112961489A (en) * | 2021-02-05 | 2021-06-15 | 深圳鑫富艺科技股份有限公司 | High-ductility TPU film and preparation method thereof |
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Application publication date: 20160817 |