CN112961489A - High-ductility TPU film and preparation method thereof - Google Patents
High-ductility TPU film and preparation method thereof Download PDFInfo
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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Abstract
The application relates to the field of electronic product films, and particularly discloses a high-ductility TPU film and a preparation method thereof, wherein the high-ductility TPU film comprises the following components in parts by weight: 80-100 parts of original membrane, 5-10 parts of nano fiber, 2-5 parts of diatomite and 3-8 parts of dispersing agent, wherein the diameter of the nano fiber is 20-30nm, and the length of the nano fiber is 0.5-2 mm; the preparation method comprises the following steps: and adding the nano-fiber, the diatomite and the dispersing agent into the molten original film together, uniformly mixing, applying positive pressure for 30min, applying negative pressure for 8h, heating for 0.5h, and coating to form a film, thereby obtaining the high-ductility TPU film. The high-ductility TPU film has the advantage of good ductility; in addition, the preparation method of the present application has an advantage of improving the ductility of the film.
Description
Technical Field
The application relates to the field of electronic product films, in particular to a high-ductility TPU film and a preparation method thereof.
Background
The TPU film is a thermoplastic elastomer, is prepared by processes of calendering, tape casting, film blowing, coating and the like on the basis of TPU granules, and is widely used as a protective film for electronic products such as mobile phones, flat plates and the like.
The invention patent application with application publication number CN107298843A discloses a modified TPU film, which takes TPU particles as raw materials, and also comprises a compatilizer, a filler, a flame retardant, natural polyphenol, epoxy resin and a light stabilizer, wherein the components in parts by weight are respectively as follows: 70-80 parts of TPU particles, 3-6 parts of compatilizer, 1-3 parts of filler, 2-4 parts of flame retardant, 5-8 parts of natural polyphenol, 10-20 parts of epoxy resin, 0.5-1.5 parts of light stabilizer and silica as filler.
In view of the above-mentioned related art, the inventors believe that since silica is a hard, brittle, poorly soluble solid, although the strength of the film can be improved, the addition to the film deteriorates the ductility of the film, so that the film is easily damaged during the processing.
Disclosure of Invention
To improve film ductility, the present application provides a high ductility TPU film and a method of making the same.
In a first aspect, the present application provides a high ductility TPU film, using the following technical solution:
a high-ductility TPU film comprises the following components in parts by weight: 80-100 parts of original membrane, 5-10 parts of nano fiber, 2-5 parts of diatomite and 3-8 parts of dispersing agent, wherein the diameter of the nano fiber is 20-30nm, and the length of the nano fiber is 0.5-2 mm.
By adopting the technical scheme, as the original film is filled with the diatomite and the nanofibers, the diatomite particles are porous and have physical adsorption property, the pores of the diatomite can adsorb the nanofibers and radially distribute in the original film around the diatomite, the dispersant enables the diatomite and the nanofibers to be uniformly distributed in the original film, the radial structures formed by a plurality of diatomite and the nanofibers are interwoven inside the original film to form a flexible net structure, and the net structure obtained by compounding the diatomite and the nanofibers is flexible and good in ductility, so that the effect of improving the ductility of the film is obtained.
Preferably, the dispersant is fatty acid polyglycol ester.
Through adopting above-mentioned technical scheme, because the adsorptivity of diatomaceous earth farine to lipid is stronger, the effort of fatty acid polyglycol ester to diatomaceous earth is stronger, is favorable to promoting diatomaceous earth evenly distributed to former membrane for network structure bulk strength distributes more evenly, is favorable to further improving the whole ductility of membrane.
Preferably, the surface of the nanofiber is coated with lipid.
Through adopting above-mentioned technical scheme, because the adsorptivity of diatomaceous earth fine powder to lipid is stronger, wrapping up lipid at nanofiber is favorable to improving the adsorption affinity of diatomaceous earth to nanofiber for during nanofiber inserts the hole of diatomaceous earth granule more easily, thereby change and form radial structure, be favorable to further improving the ductility of membrane.
Preferably, the lipid comprises the following components in parts by weight: 25-30 parts of cetyl alcohol and 70-75 parts of phospholipid, and the surface of the water-soaked nano-fiber is coated with lipid.
By adopting the technical scheme, because the cetyl alcohol has water absorption and can easily enter pores of the diatomite along with water, the compounding of the cetyl alcohol and the phospholipid can be easily coated on the surface of the nanofiber wetted by water, and the effect of further improving the ductility of the membrane is achieved.
Preferably, the lipid also comprises 10-20 parts of vaseline.
By adopting the technical scheme, the vaseline can enhance the water absorption of the cetyl alcohol, further improve the adsorbability of the lipid and the infiltrated nano-fibers and is beneficial to further improving the ductility of the membrane.
Preferably, the raw film comprises the following raw materials in parts by weight: 4-diphenylmethane diisocyanate 40-50 parts, adipic acid 30-35 parts and 1, 4-butanediol 15-25 parts.
By adopting the technical scheme, 4-diphenylmethane diisocyanate, adipic acid and 1, 4-butanediol react to obtain the polyester TPU primary membrane, and the polyester TPU primary membrane has stronger adsorption force with diatomite, so that the connection strength of the diatomite and the primary membrane is higher, the diatomite is not easy to separate from the primary membrane, and the ductility and flexibility of the membrane are improved.
Preferably, the nanofiber is a carbon nanotube fiber and/or a porous ceramic nanofiber.
By adopting the technical scheme, the carbon nanotube fiber and the porous ceramic nanofiber have high strength and contain a large number of micropores, so that the carbon nanotube fiber and the porous ceramic nanofiber have stronger adsorbability with lipid, are easier to coat on the nanofiber and are not easy to separate from the nanofiber, and the ductility of the membrane is further improved.
In a second aspect, the present application provides a method for preparing a high-ductility TPU film, which adopts the following technical scheme:
a preparation method of a high-ductility TPU film comprises the following steps of adding nanofibers, diatomite and a dispersing agent into a molten original film together, uniformly mixing, applying positive pressure for 30min, applying negative pressure for 8h, heating for 0.5h, and coating to form a film, so as to obtain the high-ductility TPU film.
By adopting the technical scheme, the diatomite, the nano fibers and the dispersing agent are added into the original film molten liquid together, so that the diatomite adsorbing nano fibers are radially distributed in the original film around the diatomite, the dispersing agent enables the diatomite and the nano fibers to be uniformly distributed in the original film, and a radial structure formed by a plurality of diatomite and nano fibers is interwoven inside the original film to form a net structure, thereby improving the ductility of the film.
Preferably, the nanofibers are first immersed in the lipid liquid, taken out and drained, and then added to the molten raw film.
By adopting the technical scheme, the lipid can be uniformly coated on the nano-fibers, so that the adsorption force between the nano-fibers and the diatomite is improved, and the ductility of the membrane is further improved.
Preferably, the nano-fibers are soaked in water, taken out and soaked in a mixed solution of cetyl alcohol, vaseline and phospholipid, taken out and drained, and then added into the molten original membrane.
By adopting the technical scheme, after the cetyl alcohol, the vaseline and the phospholipid are mixed, the cetyl alcohol, the vaseline and the phospholipid are compounded, the water absorption of the phospholipid is enhanced, after the lipid is coated on the nanofiber, when the nanofiber can be mixed with the original membrane molten liquid, the nanofiber can be easily acted with a small amount of water in the original membrane, the nanofiber can be easily mixed uniformly, and the ductility of the membrane is further improved.
In summary, the present application has the following beneficial effects:
1. because this application adopts diatomaceous earth and nanofiber complex formulation, because the pore energy of diatomaceous earth adsorbs nanofiber and is radial distribution in former membrane around diatomaceous earth, and the radial structure that many diatomaceous earth and nanofiber formed interweaves inside former membrane and forms flexible network structure, and network structure that diatomaceous earth and nanofiber complex obtained is pliable and tough and the ductility is good, obtains the effect that improves the pliability and the ductility of membrane.
2. The lipid cladding is preferably adopted on the nanofiber surface in this application, because the adsorptivity of diatomaceous earth fine powder to lipid is stronger, is favorable to improving the adsorption affinity of diatomaceous earth to nanofiber at nanofiber parcel lipid for during the hole of diatomaceous earth granule is inserted more easily to the nanofiber, thereby forms radial structure more easily, has obtained the effect of further improvement membrane's ductility.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials of the present application are obtained by home-made or commercial sources, and the specific sources are shown in table 1.
TABLE 1
| Name (R) | Specification/batch number | Source |
| Diatomite | Density of 0.47g/cm3 | Hubeixin run de chemical Co., Ltd |
| Cetyl alcohol | AR | GUANGZHOU CHENSHENG CHEMICAL TECHNOLOGY Co.,Ltd. |
| Phospholipids | AR | NINGBO DAHONGYING BIO-ENGINEERING Co.,Ltd. |
| Vaseline | AR | Guangzhou City annual bumper chemical Co Ltd |
| 4-diphenylmethane diisocyanate | AR | Kagaoyu chemical technology Co Ltd |
| Adipic acid | AR | Wuhan Jing Longgong chemical Co., Ltd |
| 1. 4-butanediol | AR | Wuhan, Dupont chemical Co Ltd |
| Polytetrahydrofuran | AR | Shanghai endi chemical Co Ltd |
| Fatty acid polyglycol ester | AR | Jiangsu Haolong chemical Co., Ltd |
| Carbon nanotube fiber | AR | Beijing Dingsheng brother science and technology Co Ltd |
| Porous ceramic nanofibers | AR | Beijing Dingsheng brother science and technology Co Ltd |
| Nano composite polypropylene fiber | AR | Beijing Dingsheng brother science and technology Co Ltd |
| Methyl amyl alcohol | AR | Shanghai Yi chemical technology Co Ltd |
| Ethanol | AR | Guangzhou Ming En petrochemical Co Ltd |
Preparation example of raw film
Preparation example 1
Weighing 4.5kg of (4-diphenylmethane diisocyanate), 2kg of (1, 4-butanediol) and 4kg of (polytetrahydrofuran) into a reaction kettle, premixing uniformly by a stirrer, adding into a double-screw reactor, reacting for 2h at 200 ℃, extruding under the pressure of 5.5MPa, carrying out underwater continuous granulation, and curing to obtain the raw film granules.
Preparation example 2
Weighing 4kg (4-diphenylmethane diisocyanate), 3kg (30-35 parts) of adipic acid and 1.5kg (1, 4-butanediol) into a reaction kettle, premixing uniformly by a stirrer, adding into a double-screw reactor, reacting for 2h at 140 ℃, extruding under the pressure of 4MPa, carrying out underwater continuous granulation, and curing to obtain the raw film granules.
Preparation example 3
Weighing 4.5kg (4-diphenylmethane diisocyanate), 3.3kg adipic acid and 2kg (1, 4-butanediol) into a reaction kettle, premixing uniformly by a stirrer, adding into a double-screw reactor, reacting for 2h at 200 ℃, extruding under the pressure of 5.5MPa, carrying out underwater continuous granulation, and curing to obtain the raw film granules.
Preparation example 4
Weighing 5kg (4-diphenylmethane diisocyanate), 3.5kg adipic acid and 2.5kg (1, 4-butanediol) into a reaction kettle, premixing uniformly by a stirrer, adding into a double-screw reactor, reacting for 2h at 250 ℃, extruding under the pressure of 7MPa, carrying out underwater continuous granulation, and curing to obtain raw film granules.
Examples
Example 1
A preparation method of a high-ductility TPU film comprises the following steps,
s1, weighing 8kg of the original film prepared in the preparation example 1, adding the original film into a reaction kettle, heating to 200 ℃, and completely dissolving the original film granules to obtain original film molten liquid;
s2, weighing 0.5kg of nano composite polypropylene fiber, 0.2kg of diatomite and 0.3kg of dispersing agent, adding the nano composite polypropylene fiber, the dispersing agent is methyl amyl alcohol, uniformly stirring, applying positive pressure for 30min and negative pressure for 8h, keeping the temperature for 0.5h, and coating to form a film to obtain the high-ductility TPU film.
Example 2
A method for preparing a high-ductility TPU film, which is different from example 1 in that in the step S1, the amount of raw film pellets added is 9 kg; in step S2, the amounts of nanofiber, diatomaceous earth, and dispersant added were 0.8kg, 0.3kg, and 0.6kg, respectively.
Example 3
A method for preparing a high-ductility TPU film, which is different from example 2 in that in the step S1, the amount of raw film pellets added is 10 kg; in step S2, the amounts of nanofiber, diatomaceous earth, and dispersant added were 1kg, 0.5kg, and 0.8kg, respectively.
Example 4
A method for preparing a high-ductility TPU film, which is different from example 2 in that the dispersant is fatty acid polyglycol ester in the S2 step.
Example 5
A preparation method of a high-ductility TPU membrane is different from that of the embodiment 2 in that in the step S2, 10kg of phospholipid is firstly dissolved in 10kg of ethanol to be diluted to obtain phospholipid diluent, then nano fibers are soaked in the liquid phospholipid diluent, and the liquid phospholipid diluent is fished out and drained and then added into the original membrane molten liquid.
Example 6
A method for preparing a TPU film with high ductility, which is different from embodiment 5 in that, in the step S2, 2.5kg of cetyl alcohol and 2kg of water are mixed uniformly to obtain an emulsion, 7.5kg of phospholipid is dissolved in 10kg of ethanol to be diluted to obtain a phospholipid diluent, and the emulsion is added into the phospholipid diluent to be mixed uniformly to obtain a lipid impregnation solution; soaking the nano-fibers in water, taking out the nano-fibers until no water drops, soaking the nano-fibers in lipid impregnation liquid, taking out the nano-fibers, draining, and adding the nano-fibers into the original membrane molten liquid.
Example 7
A method for preparing a TPU film having high ductility, which is different from example 6 in that, in the step S2, 3kg of cetyl alcohol is added to 2kg of water and mixed to obtain an emulsion, 7kg of phospholipids is dissolved in 10kg of ethanol to obtain a phospholipid diluent, and the emulsion is added to the phospholipid diluent and mixed to obtain a lipid-impregnated solution.
Example 8
A method for preparing a TPU film having high ductility, which is different from example 6 in that, in the step S2, 2.5kg of cetyl alcohol and 1kg of vaseline are mixed uniformly, then 2kg of water is added and mixed uniformly to obtain an emulsion, and the emulsion is added to a phospholipid diluent and mixed uniformly to obtain a lipid-impregnated solution.
Example 9
A method for preparing a TPU film having high ductility, which is different from example 6 in that, in the step S2, 2.5kg of cetyl alcohol and 2kg of vaseline are mixed uniformly, then 2kg of water is added and mixed uniformly to obtain an emulsion, and the emulsion is added to a phospholipid diluent and mixed uniformly to obtain a lipid-impregnated solution.
Example 10
A preparation method of a high-ductility TPU film is different from that of the embodiment 2 in that 9kg of raw film granules prepared in the preparation 2 are weighed in a reaction kettle in the step of S1, the temperature is raised to 200 ℃, and the raw film granules are completely dissolved to obtain a raw film molten liquid.
Example 11
A preparation method of a high-ductility TPU film is different from that of the embodiment 2 in that 9kg of raw film granules prepared in the preparation 3 are weighed in a reaction kettle in the step of S1, the temperature is raised to 200 ℃, and the raw film granules are completely dissolved to obtain a raw film molten liquid.
Example 12
A preparation method of a high-ductility TPU film is different from that of the embodiment 2 in that 9kg of raw film granules prepared in the preparation 4 are weighed in a reaction kettle in the step of S1, the temperature is raised to 200 ℃, and the raw film granules are completely dissolved to obtain a raw film molten liquid.
Example 13
A method for preparing a high ductility TPU film, which is different from example 2 in that the nanofibers are carbon nanotube fibers in the S2 step.
Example 14
A method for preparing a high ductility TPU film, which is different from example 2 in that in the S2 step, the nanofibers are porous ceramic nanofibers.
Example 15
A method for preparing a TPU film having high ductility, which is different from example 2 in that in the step S2, nanofibers are carbon nanotube fibers and porous ceramic nanofibers, wherein the amount of carbon nanotube fibers is 0.4kg, and the amount of porous ceramic nanofibers is 0.4 kg.
Comparative example
Comparative example 1
A method for preparing a high-ductility TPU film, which is different from example 2 in that diatomaceous earth is added in an amount of 0 in step S2.
Comparative example 2
A method for preparing a high-ductility TPU film, which is different from example 2 in that nanofibers are added in an amount of 0 in the step of S2.
Comparative example 3
A method for preparing a high ductility TPU film, which is different from example 2 in that the length of the nanofibers is 5mm in the S2 step.
Comparative example 4
A method for preparing a high ductility TPU film, which is different from example 2 in that the length of the nanofibers in step S2 is 0.3 mm.
Comparative example 5
A method for preparing a high ductility TPU film, which is different from example 2 in that the diameter of the nanofibers is 10nm in the S2 step.
Comparative example 6
A method for preparing a high ductility TPU film, which is different from example 2 in that the diameter of the nanofibers is 100nm in the S2 step.
Performance test
1. Ductility: preparing a rectangular sample with the length of 10cm, the width of 3cm and the thickness of 1mm, clamping the sample by using a tensile testing machine to perform a linear tensile test until the sample is stretched to be broken, and measuring the length L of the tested sample1cm, calculating the length change value (L) before and after the test1-10) cm, calculating the elongation: (L)1-10)/10*100％。
2. Flexibility: and adhering the prepared sample to a metal plate, bending the metal plate, folding, and observing whether the surface of the sample is cracked or cracked through a 4-time magnifier.
Test results
The results of the performance tests of the above examples are shown in table 2:
TABLE 2
The results of the above comparative performance tests are shown in table 3:
TABLE 3
Analysis of results
1. Combining example 2 and comparative examples 1-2 and tables 2-3, it can be seen that the elongation of example 2 is much greater than that of comparative examples 1 and 2, and it can be seen that the pores of diatomaceous earth can adsorb nanofibers radially distributed in the original membrane around the diatomaceous earth, and the radial structure formed by a plurality of diatomaceous earth and nanofibers interweaves inside the original membrane to form a flexible network structure, so that the addition of diatomaceous earth and nanofibers to the membrane at the same time can improve the ductility of the membrane. The film prepared in example 2 has better flexibility than the film prepared in comparative example 2, and the mesh structure woven by the nanofibers has good flexibility, which is beneficial to improving the flexibility of the film.
2. Combining examples 1-3 and Table 2, it can be seen that when the amount of nanofibers is 0.5-1kg and the amount of diatomaceous earth is 0.2-0.5kg, the ductility and flexibility of the resulting film are better.
3. It can be seen from the combination of example 2 and comparative examples 3 to 4 and tables 2 to 3 that the ductility of comparative example 3 is reduced, and it can be seen that the nanofibers having too long lengths are easily entangled with each other, so that the formed network structure is irregular, thereby making the ductility of the resulting film inferior to that of example 2. Comparative example 4 shows little change in ductility, but cracks occurred after bending, and it can be seen that the nanofibers are too short, making the radial structure much shorter, thereby deteriorating the flexibility of the resulting film.
4. As can be seen by combining example 2, comparative examples 5 to 6, and tables 2 to 3, comparative example 5 produced a film having poor ductility as compared to example 2, and it can be seen that too small a diameter of the nanofibers makes the nanofibers themselves weak and more brittle, thereby deteriorating ductility of the produced film. Comparative example 6 is less ductile than example 2, and it can be seen that the diameter of the nanofibers is too large, making it more difficult for the nanofibers to enter the pores of the diatomaceous earth to form a radial structure and thus to form a regular network structure, resulting in a film having reduced ductility.
5. As can be seen by combining examples 2-4 and tables 2-3, the ductility of the membrane prepared in example 4 is better than that of example 2, and it can be seen that after the surface of the nanofibers is coated with a layer of phospholipid, since the adsorption of the lipid by the diatomaceous earth is stronger, the adsorption of the nanofiber by the diatomaceous earth is improved by coating the lipid on the nanofibers, so that the nanofibers are easier to insert into the pores of the diatomaceous earth, and thus a radial structure is easier to form, which is beneficial to further improving the ductility of the membrane.
6. Combining example 5 with examples 6-7 and tables 2-3, it can be seen that the ductility of the films prepared in examples 6 and 7 is better than that of example 5, and it can be seen that since cetyl alcohol has water absorption property and can easily enter into the pores of diatomite, the cetyl alcohol and phospholipid compound can be easily coated on the surface of the nanofiber wetted by water, thereby further improving the ductility of the film.
7. Combining example 6 with examples 8 and 9 and tables 2 to 3, it can be seen that the ductility of the films obtained in examples 8 and 9 is better than that of example 6, and it can be seen that the further improvement of the ductility of the films is facilitated by the fact that petrolatum enhances the water absorption of cetyl alcohol.
8. As can be seen by combining examples 2 and 10 to 12 with tables 2 to 3, the polyester TPU raw film prepared in preparation examples 2 to 4 has stronger adsorption force with diatomite, so that the connection strength of the diatomite and the raw film is stronger, the diatomite is not easy to separate from the raw film, and the ductility and the flexibility of the film are improved.
9. Combining example 2 and examples 13-15 with tables 2-3, it can be seen that examples 13-15, due to the use of nanofibers having a large number of micropores, increase the adsorption of the nanofibers to lipids, so that the nanofibers are more easily coated onto the nanofibers and are less easily detached from the nanofibers, thereby further increasing the ductility of the film.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The high-ductility TPU film is characterized by comprising the following components in parts by weight: 80-100 parts of original membrane, 5-10 parts of nano fiber, 2-5 parts of diatomite and 3-8 parts of dispersing agent, wherein the diameter of the nano fiber is 20-30nm, and the length of the nano fiber is 0.5-2 mm.
2. A high ductility TPU film as claimed in claim 1, wherein: the dispersant is fatty acid polyglycol ester.
3. A high ductility TPU film as claimed in claim 1, wherein: the surface of the nanofiber is coated with lipid.
4. A high ductility TPU film as claimed in claim 3, wherein: the lipid comprises the following components in parts by weight: 25-30 parts of cetyl alcohol and 70-75 parts of phospholipid, and the surface of the water-soaked nano-fiber is coated with lipid.
5. The high ductility TPU film of claim 4, wherein the lipid further comprises vaseline 10-20 parts.
6. The high ductility TPU film of claim 1, wherein the raw film is polymerized from the following raw materials in parts by weight: 4-4，40-50 parts of diphenylmethane diisocyanate, 30-35 parts of adipic acid and 15-25 parts of 1, 4-butanediol.
7. A high ductility TPU film as claimed in any one of claims 1 to 6 wherein the nanofibers are carbon nanotube fibers and/or porous ceramic nanofibers.
8. A method for preparing the TPU film with high ductility as claimed in any one of claims 1 to 2, comprising the steps of adding nanofibers, diatomaceous earth and a dispersing agent together into a molten original film, mixing uniformly, applying positive pressure for 30min and negative pressure for 8h, heating for 0.5h, and coating to form a film, thereby obtaining the TPU film with high ductility.
9. The high ductility TPU film of claim 8, wherein the nanofibers are first dipped into the lipid liquid, removed and drained, and then added to the molten raw film.
10. The high ductility TPU film of claim 8, wherein the nanofibers are first soaked in water, then dipped into a blended solution of cetyl alcohol, petrolatum and phospholipids, and then added to the molten original film after being drained.
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