CN114347521A - Preparation method of non-oriented PVF film - Google Patents
Preparation method of non-oriented PVF film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000002904 solvent Substances 0.000 claims abstract description 68
- 239000011347 resin Substances 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 238000005266 casting Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 17
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 238000010345 tape casting Methods 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004513 sizing Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 claims description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 73
- 229920002620 polyvinyl fluoride Polymers 0.000 description 69
- 239000012528 membrane Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
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- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
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Abstract
The invention discloses a preparation method of a non-oriented PVF film, which comprises the following steps: adding PVF resin and a latent solvent into an extruder, mixing and melting in the extruder, extruding, casting to form a film, obtaining a wet film, and removing the latent solvent from the wet film through a graded water bath under the control of the tension of 100-300N to obtain the non-oriented PVF film. The PVF film prepared by the method has the advantages of good flatness, high stretching degree, simple film preparation process, solvent recycling, low energy consumption, high production efficiency and less three wastes.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a preparation method of a non-oriented PVF film and the non-oriented PVF film obtained by the preparation method.
Background
Polyvinyl fluoride (PVF) is a kind of polymer synthesized by the derivatives of ethylene with hydrogen atom replaced by fluorine atom, and the repeating structural unit of its molecular formula is (-CH)2CHF-), which is a kind of fluororesin with the lowest density and fluorine content and the lower cost. The PVF film product has the excellent characteristics of fluorine materials, such as good corrosion resistance, wear resistance, self-lubricating property, dielectric property, ultraviolet ray resistance, weather resistance and the like, and is widely applied to the fields of building outer packaging, solar cells, anticorrosion covering materials and the like.
PVF films exist in both oriented and non-oriented forms. The oriented PVF film is obtained by dispersing PVF resin in a latent solvent for melt processing and then performing biaxial tension from the longitudinal direction and the transverse direction, and the mechanical property of the oriented PVF film is enhanced; the non-oriented PVF film is a non-stretched non-oriented flat extruded film obtained by adopting a tape casting process, and compared with the oriented PVF film, the non-oriented PVF film is easier to form and has better compatibility.
Non-oriented PVF films have the advantages of good flexibility, low tensile strength, high elongation at break and the like, and are widely used in occasions with low requirements for mechanical properties, including aircraft interiors, sunshades, body side moldings, wallcoverings, building panels and thermoplastic laminates.
U.S. patent No. 5972472 discloses a process for preparing a controlled gloss fluoropolymer film by cast coating a fluoropolymer dispersion onto a carrier substrate coated with an inert particulate material, coagulating, drying to devolatilize, and then peeling from the carrier substrate to produce a controlled gloss or matte fluoropolymer film. The inert particles on the carrier substrate are easy to gather and agglomerate to pollute the casting surrounding environment, a high-quality casting film is difficult to prepare, meanwhile, the uniformity of the inert particle material coated on the carrier substrate is difficult to control, and the prepared film is easy to form defects and even breaks the film.
US patent 4883716 discloses a process for preparing a fluorine-containing film by coating a fluoropolymer resin onto a support, which process comprises: (a) preparing a fluoropolymer dispersion; (b) dipping the carrier tape through the dispersion to form a dispersion coating on the carrier tape; (c) passing the carrier tape coated with the dispersion coating through a meter to remove excess dispersion; (d) drying the metered coating carrier to remove the solvent from the coating; (e) the coating is dried by heating to coagulate the dispersion into a film. The quality of the fluorine-containing thin film prepared by the method is easily influenced by the fineness of polymer particles, the uniformity of dispersion and large-particle auxiliary agent particles, and defects are easily formed.
At present, a non-oriented PVF film is usually prepared by a coating method, but the coating method has high requirements on material state, equipment cleanliness and the like, the prepared non-oriented PVF film is uneven and easy to become brittle, defects are easy to form and cause film breaking, and in addition, the existing preparation method of the non-oriented PVF film also has the problems of high solvent requirement, high energy consumption, low production efficiency and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a non-oriented PVF film, which has the advantages of good flatness and high stretching degree of the obtained PVF film, simple film preparation process, solvent recycling, low energy consumption, high production efficiency and less three wastes.
The invention is realized by the following technical scheme:
a preparation method of a non-oriented PVF film comprises the following steps: adding PVF resin and a latent solvent into an extruder, mixing and melting in the extruder, extruding, casting to form a film, obtaining a wet film, and removing the latent solvent from the wet film through a graded water bath under the control of the tension of 100-300N to obtain the non-oriented PVF film.
The PVF resin and the latent solvent are prepared into dispersion slurry and added into an extruder or the PVF resin and the latent solvent are respectively added into the extruder.
Specifically, the PVF resin and the latent solvent are added into an extruder, the mixture is extruded after being mixed and melted in the extruder, a wet membrane is obtained after the film is formed through tape casting of a casting roll, the latent solvent is removed from the wet membrane through a grading water bath under the control of the tension of 100-300N, and the non-oriented PVF film is obtained after devolatilization and sizing through a drying tunnel.
Because the wet film sheet formed by extrusion casting has internal stress, the film is easy to deform in the process of removing the latent solvent through the grading water bath, and the flatness and the uniformity of the film can be effectively controlled under the control of tension; on the other hand, the retraction proportion of the wet diaphragm in the water bath tank is controlled by regulating and controlling the tension, so as to achieve the purpose of controlling the thickness stability of the film.
The temperature of the casting roller is 30-60 ℃; the thickness of the wet film sheet is 20-60 mu m.
The drying channel further devolatilizes and anneals the wet film, eliminates the internal stress of the film and improves the thickness stability of the film. The temperature of the drying tunnel is 140-200 ℃, and the treatment time of the drying tunnel is 5-30 min.
The invention adopts the water bath to extract and remove the latent solvent, not only has low energy consumption, but also can recycle the water bath, is convenient for recycling the latent solvent and greatly reduces waste gas and waste water.
The extraction and desolvation of the grading water bath can effectively desolvation only by controlling the processing time and the tension of the grading water bath.
The grading water bath is divided into three stages, and the water bath at each stage is communicated with each other. Specifically, each stage of water bath can be respectively provided with a valve, the installation positions of the water bath are gradually increased, or each stage of water bath is respectively provided with a delivery pump, so that water in the water bath with the low solvent weight content at the rear section is discharged into the water bath with the high solvent weight content at the front section, and the water bath with the high solvent weight content can be recycled after the solvent content reaches a certain concentration, so that the water bath can be repeatedly used, and the waste water is reduced.
The water bath temperature of the water bath is 25-45 ℃; the mass percentages of the solvents in the first-stage water bath, the second-stage water bath and the third-stage water bath are respectively 0-40%, 0-20% and 0-5%; the residence time of the wet diaphragm in the first-stage water bath, the second-stage water bath and the third-stage water bath is 10-60 seconds respectively.
The cosolvent is a conventional cosolvent. Preferably, the latent solvent is selected from at least one of gamma-butyrolactone, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, propylene carbonate, hexamethylphosphoramide; more preferably, the latent solvent is selected from at least one of gamma-butyrolactone, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone. The mass ratio of the PVF resin to the latent solvent is 1: 1.1-1: 2.5.
specifically, when the PVF resin and the latent solvent are formulated into a dispersion slurry, the mass ratio of the PVF resin to the latent solvent is 1: 1.4-1: 2.5.
when the PVF resin and the latent solvent are separately fed into the extruder, the amount of latent solvent required is greatly reduced. The mass ratio of the PVF resin to the latent solvent is 1: 1.1-1: 1.4.
the PVF resin is added into an extruder through a feeding screw, and the feeding speed is 10-40 g/min; the latent solvent is pumped into an extruder through a solvent delivery pump, and the delivery speed is 10-60 g/min; the ratio of the PVF resin feeding speed to the latent solvent conveying speed is 1: 1-1: 2.
Further, the PVF resin is in a powder state, and the preparation method of the non-oriented PVF film comprises the following steps: adding PVF resin powder into an extruder through a feeding screw, pumping a latent solvent into the extruder through a solvent delivery pump, mixing, dispersing and melting the PVF resin powder and the latent solvent in the extruder, extruding the mixture through a flat extrusion die head, carrying out tape casting on the mixture through a casting roll to form a film, obtaining a wet film, cooling the wet film through a cooling roll, removing the latent solvent from the wet film through a graded water bath under the control of the tension of 100-300N, and carrying out devolatilization and sizing through a drying tunnel to obtain the non-oriented PVF film.
The non-oriented PVF film prepared by the preparation method of the non-oriented PVF film has the thickness of 15-50 mu m, the tensile strength of 30-40 MPa, the elongation at break of 200-300% and the haze of 5-25%. The non-oriented PVF film has the advantages of good flexibility and flatness, high elongation at break, easiness in forming and good compatibility.
Compared with the prior art, the invention has the beneficial effects that:
(1) the PVF resin and the latent solvent are fed separately and continuously, so that the needed latent solvent is greatly reduced, the preparation process is simple, the limitations of biaxial stretching equipment and the process are overcome, and the PVF film with thinner thickness can be continuously and stably produced;
(2) the latent solvent is removed by utilizing the grading water bath, so that the energy consumption is low, the water bath can be recycled, the solvent can be conveniently recycled, and the generation of waste gas and waste water is greatly reduced;
(3) the non-oriented PVF film prepared by the method has the advantages of good flexibility and flatness, high elongation at break, easiness in forming and good compatibility.
Drawings
FIG. 1 illustrates a process for preparing a non-oriented PVF film according to a preferred embodiment of the present invention;
wherein the figures include the following reference numerals:
1. a solvent delivery pump; 2. a feed screw; 3, a first-stage water bath; 4. a second stage water bath; 5. a third stage water bath; 6. and (4) a drying channel.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
PVF resin powder is added into a double-screw extruder at a feeding speed of 12g/min through a feeding screw rod (2), N-dimethylformamide is pumped into the double-screw extruder at a conveying speed of 14g/min through a solvent conveying pump (1), the PVF resin powder and the N, N-dimethylformamide are mixed, dispersed and melted in the double-screw extruder, then are extruded through a horizontal extrusion die head, then are cast through a casting roll at 40 ℃ to obtain a wet membrane with the thickness of 30 mu m, the wet membrane is cooled through a cooling roll, and then passes through a grading water bath sequentially under the tension control of 150N to extract and remove latent solvent, the water temperature of the water bath is controlled to be 25 ℃, and the initial solvent mass percentage content in a first-stage water bath (3), a second-stage water bath (4) and a third-stage water bath (5) is respectively 0%, 0% and 0%, the retention time is respectively 10s, 10s and 10s, and finally, the further devolatilization and shaping are carried out through a drying tunnel (6), the temperature of the drying tunnel (6) is controlled at 150 ℃, the processing time is 20min, and finally the non-oriented PVF film with the thickness of 18 mu m is prepared.
Example 2
PVF resin powder is added into a double-screw extruder at a feeding speed of 20g/min through a feeding screw rod (2), meanwhile, gamma-butyrolactone is pumped into the double-screw extruder at a conveying speed of 28g/min through a solvent conveying pump (1), the PVF resin powder and N, N-dimethylformamide are mixed, dispersed and melted in the double-screw extruder, extruded through a horizontal extrusion die head, cast through a casting roll at 50 ℃ to obtain a wet membrane with the thickness of 40 mu m, the wet membrane is cooled through a cooling roll, and then passes through a grading water bath successively under the control of 200N tension to extract and remove latent solvent, the water temperature of the water bath is controlled at 30 ℃, the initial solvent mass percentage content in a first-stage water bath (3), a second-stage water bath (4) and a third-stage water bath (5) is respectively 10%, 10% and 5%, and the retention time is respectively 20s, 15s and 20s, and finally further devolatilizing and shaping through a drying tunnel (6), wherein the temperature of the drying tunnel (6) is controlled at 190 ℃, the treatment time is 10min, and finally the non-oriented PVF film with the thickness of 18 mu m is prepared.
Example 3
Adding PVF resin powder into a double-screw extruder at a feeding speed of 25g/min through a feeding screw rod (2), pumping gamma-butyrolactone into the double-screw extruder at a conveying speed of 35g/min by using a solvent conveying pump (1), mixing, dispersing and melting the PVF resin powder and N, N-dimethylformamide in the double-screw extruder, extruding the mixture through a horizontal extrusion die head, casting the mixture through a casting roll at 55 ℃ to obtain a wet membrane with the thickness of 50 mu m, cooling the wet membrane through a cooling roll, sequentially passing through a grading water bath under the tension control of 250N to extract and remove latent solvent, controlling the water temperature of the water bath at 40 ℃, controlling the initial solvent mass percentage content in a first-stage water bath (3), a second-stage water bath (4) and a third-stage water bath (5) to be 20%, 15% and 2% respectively, and controlling the retention time to be 40s respectively, 50s and 20s, and finally further devolatilizing and shaping through a drying tunnel (6), wherein the temperature of the drying tunnel (6) is controlled at 170 ℃, the treatment time is 15min, and finally the non-oriented PVF film with the thickness of 35 mu m is prepared.
Example 4
PVF resin powder is added into a double-screw extruder at a feeding speed of 40g/min through a feeding screw rod (2), N-dimethylformamide is pumped into the double-screw extruder at a conveying speed of 45g/min through a solvent conveying pump (1), the PVF resin powder and the N, N-dimethylformamide are mixed, dispersed and melted in the double-screw extruder, then are extruded through a horizontal extrusion die head, then are cast through a casting roll at 45 ℃ to obtain a wet membrane with the thickness of 60 mu m, the wet membrane is cooled through a cooling roll, and then sequentially passes through a grading water bath under the tension control of 300N to extract and remove latent solvent, the water temperature of the water bath is controlled to be 35 ℃, and the initial solvent mass percentage content in a first-stage water bath (3), a second-stage water bath (4) and a third-stage water bath (5) is respectively 35%, 20% and 2%, the retention time is respectively 50s, 30s and 50s, and finally, the further devolatilization and shaping are carried out through a drying tunnel (6), the temperature of the drying tunnel (6) is controlled at 160 ℃, the processing time is 25min, and finally the non-oriented PVF film with the thickness of 48 mu m is prepared.
Example 5
The film formulation and process of example 5 are the same as example 1 except that: the wet film in example 5 was extracted in a water bath to remove the latent solvent, and the water bath was a bath water bath.
Comparative example 1
Dispersing 2kg of PVF resin in 4kg of gamma-butyrolactone at a high speed, carrying out melt extrusion on the prepared PVF dispersoid through a double-screw extruder, a filter, a melt metering pump and a casting die head, carrying out sheet casting through a casting roll at 40 ℃, cooling a membrane through a cooling roll, carrying out longitudinal stretching (temperature: 135 ℃, stretching ratio: 2.5) and transverse stretching (temperature: 150 ℃, stretching ratio: 3), devolatilizing and shaping the prepared PVF film through a drying tunnel under continuous tension, controlling the temperature at 190 ℃, and treating for 10min to finally prepare the oriented PVF film with the thickness of 35 mu m.
The PVF films prepared in the embodiments 1-5 and the comparative example 1 are subjected to performance test, and the test method mainly comprises the following steps:
(1) the thickness is determined according to GB/6672-2001;
(2) tensile strength and elongation at break were measured according to GB/T1040.3-2006;
(3) film shrinkage: measuring the size change rate before and after heat treatment for 30min at 150 ℃;
(4) haze test: measured according to the standard ASTM D1003-13.
TABLE 1 test results of films obtained in examples 1 to 5 and comparative example 1
As can be seen from table 1, after the wet membranes in examples 1 to 5 are subjected to extraction and desolvation by a graded water bath, the solvent content in the membranes is less than 10%, the surfaces of the finally prepared PVF films are flat and uniform, the thickness is controllable, the thermal shrinkage is less than 3%, the tensile strength is higher than 35MPa, and the elongation at break is greater than 200%; comparative example 1 is a shaped PVF film prepared after biaxial stretching, not only is the required latent solvent content high (mass ratio of solvent to PVF resin is greater than 1.4), when a thinner PVF film is prepared, especially a PVF film smaller than 20 μm, biaxial stretching easily causes film rupture and the yield is low, but also latent solvent is removed by drying tunnel heat treatment during film making, the required energy consumption is large, a large amount of waste gas is generated, in addition, the oriented PVF film in comparative example 1 is higher in tensile strength than the non-oriented PVF films in examples 1 to 5, but the elongation at break is relatively low, while the non-oriented PVF films in examples 1 to 5 are easier to apply and form and good in compatibility.
Claims (10)
1. A preparation method of a non-oriented PVF film is characterized by comprising the following steps: the preparation method comprises the following steps: adding PVF resin and a latent solvent into an extruder, mixing and melting in the extruder, extruding, casting to form a film, obtaining a wet film, and removing the latent solvent from the wet film through a graded water bath under the control of the tension of 100-300N to obtain the non-oriented PVF film.
2. The method of making a non-oriented PVF film of claim 1, wherein: the PVF resin and the latent solvent are prepared into dispersion slurry and added into an extruder or the PVF resin and the latent solvent are respectively added into the extruder.
3. The method of making a non-oriented PVF film of claim 1, wherein: and (3) carrying out tape casting on the film by using a tape casting roller to form a film to obtain a wet film, removing the latent solvent from the wet film by using a grading water bath under the control of the tension of 100-300N, and carrying out devolatilization and sizing by using a drying tunnel to obtain the non-oriented PVF film.
4. A method of making a non-oriented PVF film according to any of claims 1-3, wherein: the grading water bath is divided into three stages, and the water bath at each stage is communicated with each other.
5. The method of making a non-oriented PVF film of claim 4, wherein: the water bath temperature of the water bath is 25-45 ℃; the mass percentages of the solvents in the first-stage water bath, the second-stage water bath and the third-stage water bath are respectively 0-40%, 0-20% and 0-5%; the residence time of the wet diaphragm in the first-stage water bath, the second-stage water bath and the third-stage water bath is 10-60 seconds respectively.
6. The method of making a non-oriented PVF film of claim 1, wherein: the latent solvent is at least one of gamma-butyrolactone, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, propylene carbonate and hexamethylphosphoramide.
7. The method of making a non-oriented PVF film of claim 2, wherein: the PVF resin is added into an extruder through a feeding screw, and the feeding speed is 10-40 g/min; the latent solvent is pumped into an extruder through a solvent delivery pump, and the delivery speed is 10-60 g/min; the ratio of the PVF resin feeding speed to the latent solvent conveying speed is 1: 1-1: 2.
8. A method of making a non-oriented PVF film according to claim 3, wherein: the temperature of the casting roller is 30-60 ℃; the thickness of the wet film sheet is 20-60 mu m.
9. A method of making a non-oriented PVF film according to claim 3, wherein: the temperature of the drying tunnel is 140-200 ℃, and the treatment time of the drying tunnel is 5-30 min.
10. A non-oriented PVF film produced by the method of any one of claims 1 to 9, wherein: the thickness of the non-oriented PVF film is 15-50 mu m, the tensile strength is 30-40 MPa, the elongation at break is 200-300%, and the haze is 5-25%.
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CN101168294A (en) * | 2006-10-27 | 2008-04-30 | 北京化工大学 | Preparation of polyvinyl fluoride thin film by fusion extrusion casting method |
CN101820987A (en) * | 2007-10-11 | 2010-09-01 | 3M创新有限公司 | Microporous membranes having a relatively large average pore size and methods of making the same |
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CN102276948A (en) * | 2010-09-03 | 2011-12-14 | 中化蓝天集团有限公司 | Preparation method of biaxially stretched polyvinyl fluoride film |
CN102241832A (en) * | 2011-05-14 | 2011-11-16 | 中材科技股份有限公司 | Polyolefin film and preparation method thereof |
CN103978707A (en) * | 2014-04-17 | 2014-08-13 | 常州纺织服装职业技术学院 | Washing technology of 1,3,4-oxadiazole acid-containing wet casting film |
CN106700350A (en) * | 2015-11-13 | 2017-05-24 | 浙江蓝天环保高科技股份有限公司 | Preparation method for polyvinyl fluoride film with good weatherability |
CN108284627A (en) * | 2018-01-30 | 2018-07-17 | 中国久远高新技术装备公司 | A kind of wet method curtain coating coagulation forming method for manufacturing thin film |
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