CN111016039B - Preparation process of bending-resistant polytetrafluoroethylene film - Google Patents
Preparation process of bending-resistant polytetrafluoroethylene film Download PDFInfo
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- CN111016039B CN111016039B CN201911312217.5A CN201911312217A CN111016039B CN 111016039 B CN111016039 B CN 111016039B CN 201911312217 A CN201911312217 A CN 201911312217A CN 111016039 B CN111016039 B CN 111016039B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/006—Pressing and sintering powders, granules or fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
- B29K2027/18—PTFE, i.e. polytetrafluorethene, e.g. ePTFE, i.e. expanded polytetrafluorethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention provides a preparation process of a bending-resistant polytetrafluoroethylene film, which comprises the following steps: sieving polytetrafluoroethylene resin powder by a 10-mesh screen, and then carrying out compression molding, sintering and turning to obtain a turned film; and heating the turned film to be molten and pressurized, then stopping heating, and rapidly cooling to room temperature by using cold water under the condition of keeping the pressure unchanged to prepare the bending-resistant polytetrafluoroethylene film. The preparation method is simple, can obviously improve the bending resistance of the polytetrafluoroethylene film on the premise of not damaging the properties of the polytetrafluoroethylene film, such as tensile strength, elongation and the like, has MIT bending resistance times of more than 400 thousands times, and has better bending resistance.
Description
Technical Field
The invention relates to a preparation process of a bending-resistant polytetrafluoroethylene film, and belongs to the technical field of processing and manufacturing of films.
Background
Polytetrafluoroethylene films are commonly used in capacitor dielectrics for wire insulation, electrical instrument insulation, gaskets, pumps, diaphragms, and the like. The existing polytetrafluoroethylene film is made of polytetrafluoroethylene materials, and has excellent comprehensive properties such as high temperature resistance, corrosion resistance, non-adhesiveness, self-lubrication, excellent dielectric property, very low friction coefficient and the like due to the special properties of the polytetrafluoroethylene materials used in the film.
The polytetrafluoroethylene film is usually made of polytetrafluoroethylene resin through die pressing, sintering, cooling to form a blank, turning and rolling. The polytetrafluoroethylene film processed by the common method is poor in bending resistance, and tiny gaps are generated in the frequent bending use process of the film, so that the service life and the safety and reliability of the product are influenced. The polytetrafluoroethylene film is required to have high bending resistance for related parts such as pumps, corrugated pipes, diaphragms and the like, and the requirements for indexes such as safety performance, bending performance and the like of the polytetrafluoroethylene film are higher and higher along with the development of the technology, while the polytetrafluoroethylene film prepared by the common method is difficult to meet the requirements. For example, chinese patent document CN109203525A discloses a process for manufacturing a high-strength polytetrafluoroethylene film, which comprises the following steps: (1) raw material sieving, (2) compression molding, (3) sintering, (4) turning, and 5) melt stretching. The polytetrafluoroethylene film obtained by the invention has higher tensile strength through melt stretching, but has poor flexibility and bending resistance, and can not meet the requirement of high bending resistance. Therefore, a method for preparing a polytetrafluoroethylene film having high bending resistance is urgently needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation process of a bending-resistant polytetrafluoroethylene film. The preparation method is simple, can obviously improve the bending resistance of the polytetrafluoroethylene film on the premise of not damaging the properties of the polytetrafluoroethylene film, such as tensile strength, elongation and the like, has MIT bending resistance times of more than 400 thousands times, and has better bending resistance.
Description of terms:
room temperature: having the meaning known in the art, i.e. 25. + -. 5 ℃.
The technical scheme of the invention is as follows:
a preparation process of a bending-resistant polytetrafluoroethylene film comprises the following steps:
(1) sieving polytetrafluoroethylene resin powder by a 10-mesh screen, and then carrying out compression molding, sintering and turning to obtain a turned film;
(2) and heating the turned film to be molten and pressurized, then stopping heating, and rapidly cooling to room temperature by using cold water under the condition of keeping the pressure unchanged to prepare the bending-resistant polytetrafluoroethylene film.
Preferably, in step (1), the polytetrafluoroethylene resin powder is commercially available or prepared according to the prior art.
Preferably, in step (1), the polytetrafluoroethylene resin powder has a particle size of 10 to 50 μm.
Preferably, in step (1), the polytetrafluoroethylene resin has a standard relative density (SSG) of 2.140 to 2.180.
Preferably, in the step (1), the compression molding is carried out at a compression rate of 10-100mm/min, at room temperature and under a pressure of 10-50MPa for 3-30 min; preferably, the compression molding is carried out at a compression rate of 10-30mm/min, under a pressure of 20-30MPa and under a pressure-holding time of 10-20 min.
Preferably, in step (1), the compression molding comprises the steps of: increasing the pressure to 3-8MPa at the speed of 10-100mm/min at room temperature, returning the press, increasing the pressure to 10-50MPa at the speed of 10-100mm/min after 3-6 seconds, and maintaining the pressure for 3-30 min.
According to the invention, the feeding is uniform in compression molding, so that the raw materials are uniformly scattered and distributed in the molding die, and the uniform density of the blank is facilitated. The pressurizing rate is preferably slowed as much as possible in the compression molding and pressurizing process, and the blank must be deflated in the compression process, so that the blank can be prevented from generating interlayer and bubbles, wherein deflation refers to the process of relaxing the pressure when the pressure is increased to a certain stage, retracting the press, re-pressurizing to the required pressure after a few seconds and maintaining the pressure, so as to complete the pressure transmission and facilitate the clearance elimination.
Preferably, in step (1), the sintering conditions are: heating from room temperature to 290 ℃ at the speed of 1-5 ℃/min, preserving heat at 290 ℃ for 5-15min, heating from 290 ℃ to 360-390 ℃ at the speed of 1-3 ℃/min, preserving heat for 6-10h, finally cooling to 290 ℃ at the speed of 1-3 ℃/min, and naturally cooling from 290 ℃ to room temperature. Preferably, the sintering conditions are as follows: heating from room temperature to 290 deg.C at 3 deg.C/min, maintaining at 290 deg.C for 10min, heating from 290 deg.C to 380 deg.C at 1 deg.C/min, maintaining for 8h, cooling to 290 deg.C at 1 deg.C/min, and naturally cooling from 290 deg.C to room temperature.
According to the invention, sintering is carried out by heating the blank to a temperature above the melting point of polytetrafluoroethylene, maintaining the temperature for a certain period of time, gradually changing polymer molecules from crystalline to amorphous, fusing the dispersed single resin particles into a continuous whole by interdiffusion, and then reducing the temperature to a temperature below the melting point at a certain cooling rate, so that the polymer molecules are transformed from amorphous to crystalline. The porosity and crystallinity of the product can be influenced by the heating mode and rate, the sintering temperature, the cooling rate and the like, and further the physical, mechanical and electrical properties of the product are influenced.
Preferably, in step (1), after sintering and before turning, the blank obtained by sintering is subjected to heat preservation at 100 ℃ for 1-5 hours. In order to ensure the quality of the film, the sintered blank is placed in an oven for heat preservation at 100 ℃ before turning, and is cut after heat is soaked in the blank, so that a smooth cutting surface is obtained, and better performance stability is kept.
Preferably, in the step (2), the heating is carried out until the melting is finished, the heating is maintained for 1-100min, and the pressurizing pressure is controlled to be 0.1-10 MPa; preferably, the heating temperature is controlled to be above 330 ℃, the heating is maintained for 5-15min after the melting, and the pressure of the pressurization is controlled to be 0.1-1 MPa; further preferably, the heating temperature is 350-.
According to the invention, in the step (2), the temperature of the cold water is preferably 0-20 ℃.
Preferably, in step (2), the polytetrafluoroethylene film has a thickness of 0.1 to 1.0 mm.
The invention has the following technical characteristics and beneficial effects:
1. the key step of the invention is step (2), which can improve the bending resistance of the polytetrafluoroethylene film. Heating to melt the polytetrafluoroethylene film, and pressurizing in a molten state to make the intermolecular pores of the polymer smaller and arranged tightly, thereby reducing defects; the heating temperature needs to be proper, and too high temperature can cause the decomposition of the polytetrafluoroethylene, thereby influencing the mechanical properties such as the bending resistance and the like of the final polyethylene film; the pressurizing pressure needs to be proper, the smoothness of the surface of the film can be influenced when the pressurizing pressure is too high, and the pore reducing effect cannot be realized when the pressurizing pressure is too low. On the other hand, the crystallinity of the polytetrafluoroethylene film is reduced by rapidly cooling the polytetrafluoroethylene film with cold water in a molten state under a constant pressure. Through the two measures, the bending resistance of the polytetrafluoroethylene film can be greatly improved, and the mechanical properties of the polytetrafluoroethylene film, such as tensile strength, elongation and the like, are not damaged.
2. The polytetrafluoroethylene film with good bending resistance can be prepared only by combining specific raw materials with specific procedures; the steps and conditions of the invention supplement each other, and the lack of one is not necessary. The MIT bending-resistant times of the polytetrafluoroethylene film can reach more than 440 ten thousand times, which shows that the polytetrafluoroethylene film has better bending-resistant performance. In addition, the invention applies pressure in the state of melting the polytetrafluoroethylene to reduce the content of the gaps in the film to the maximum extent, reduces the defects and has certain improvement effect on other mechanical properties, namely the invention improves the bending resistance of the polyethylene film and simultaneously has higher voltage resistance, excellent dielectric property, high temperature resistance, wear resistance, weather resistance and the like. Therefore, the polytetrafluoroethylene film prepared by the invention can be used for manufacturing device parts requiring high bending resistance, such as high-grade insulating wrapping, pumps, corrugated pipes, diaphragms and the like in the electromechanical and electronic industries, and can completely meet the requirements of the market on the bending-resistant polytetrafluoroethylene film.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
In the examples, the polytetrafluoroethylene resin DF-161, which has a particle size of 20-30um and SSG of 2.150-2.180, is commercially available from Doonto corporation.
Example 1
A preparation process of a bending-resistant polytetrafluoroethylene film comprises the following steps:
(1) sieving raw materials: sieving the polytetrafluoroethylene resin DF-161 by a 10-mesh sieve for later use;
(2) compression molding: loading the sieved polytetrafluoroethylene resin DF-161 into a mold, boosting the pressure to 5MPa at the speed of 15mm/min at room temperature, withdrawing the press, boosting the pressure to 25MPa at the speed of 15mm/min again after 4-5 seconds, maintaining the pressure for 15min, and taking out for later use;
(3) and (3) sintering: putting the molded product obtained in the step (2) into a sintering furnace, heating from room temperature to 290 ℃ at the speed of 3 ℃/min, preserving heat at 290 ℃ for 10min, heating from 290 ℃ to 380 ℃ at the speed of 1 ℃/min, preserving heat at 380 ℃ for 8h, then cooling from 380 ℃ to 290 ℃ at the speed of 1 ℃/min, naturally cooling from 290 ℃ to room temperature, and taking out for later use;
(4) turning: preserving the temperature of the sintered product obtained in the step (3) at 100 ℃ for 3h, and turning on a lathe to obtain a turned film;
(5) and (3) heat treatment: and (3) shearing the turned film obtained in the step (4) to a certain size, putting the turned film into a mold, putting the mold on a high-temperature press, melting the film at the temperature of 380 ℃, applying pressure to 0.3MPa, keeping the temperature at the temperature of 380 ℃ and the pressure of 0.3MPa for 5min, stopping heating, rapidly cooling the film to below 50 ℃ by cold water (7 ℃) under the condition of continuously pressurizing the film at the pressure of 0.3MPa, and finally taking out the film from the mold to obtain the bending-resistant polytetrafluoroethylene film with the thickness of 0.5 mm.
Example 2
A preparation process of a bending-resistant polytetrafluoroethylene film comprises the following steps:
(1) sieving raw materials: sieving the polytetrafluoroethylene resin DF-161 by a 10-mesh sieve for later use;
(2) compression molding: loading the sieved polytetrafluoroethylene resin DF-161 into a mold, boosting the pressure to 5MPa at the rate of 20mm/min at room temperature, retracting the press, boosting the pressure to 27MPa at the rate of 20mm/min again after 4-5 seconds, maintaining the pressure for 15min, and taking out for later use;
(3) and (3) sintering: putting the molded product obtained in the step (2) into a sintering furnace, heating from room temperature to 290 ℃ at the speed of 3 ℃/min, preserving heat at 290 ℃ for 10min, heating from 290 ℃ to 380 ℃ at the speed of 1 ℃/min, preserving heat at 380 ℃ for 8h, then cooling from 380 ℃ to 290 ℃ at the speed of 1 ℃/min, naturally cooling from 290 ℃ to room temperature, and taking out for later use;
(4) turning: preserving the temperature of the sintered product obtained in the step (3) at 100 ℃ for 3h, and turning on a lathe to obtain a turned film;
(5) and (3) heat treatment: and (3) cutting the turned film obtained in the step (4) to a certain size, putting the turned film into a mold, putting the mold on a high-temperature press, melting the film at the temperature of 370 ℃, applying pressure to 0.5MPa, keeping the temperature at the temperature of 370 ℃ and the pressure at the pressure of 0.5MPa for 10min, stopping heating, rapidly cooling the film to below 50 ℃ by cold water (7 ℃) under the condition of continuously pressurizing 0.5MPa, and finally taking out the film from the mold to obtain the bending-resistant polytetrafluoroethylene film with the thickness of 0.5 mm.
Example 3
A preparation process of a bending-resistant polytetrafluoroethylene film comprises the following steps:
(1) sieving raw materials: sieving the polytetrafluoroethylene resin DF-161 by a 10-mesh sieve for later use;
(2) compression molding: loading the sieved polytetrafluoroethylene resin DF-161 into a mold, boosting the pressure to 5MPa at the speed of 30mm/min at room temperature, withdrawing the press, boosting the pressure to 20MPa at the speed of 30mm/min again after 4-5 seconds, maintaining the pressure for 15min, and taking out for later use;
(3) and (3) sintering: putting the molded product obtained in the step (2) into a sintering furnace, heating from room temperature to 290 ℃ at the speed of 3 ℃/min, preserving heat at 290 ℃ for 10min, heating from 290 ℃ to 380 ℃ at the speed of 1 ℃/min, preserving heat at 380 ℃ for 8h, then cooling from 380 ℃ to 290 ℃ at the speed of 1 ℃/min, naturally cooling from 290 ℃ to room temperature, and taking out for later use;
(4) turning: preserving the temperature of the sintered product obtained in the step (3) at 100 ℃ for 3h, and turning on a lathe to obtain a turned film;
(5) and (3) heat treatment: and (3) shearing the turned film obtained in the step (4) to a certain size, putting the turned film into a mold, putting the mold on a high-temperature press, melting the film at the temperature of 360 ℃, applying pressure to 0.8MPa, keeping the temperature at the temperature of 360 ℃ and the pressure at the pressure of 0.8MPa for 15min, stopping heating, rapidly cooling the film to below 50 ℃ by cold water (7 ℃) under the condition of continuously pressurizing the film at the pressure of 0.8MPa, and finally taking out the film from the mold to obtain the bending-resistant polytetrafluoroethylene film with the thickness of 0.5 mm.
Comparative example 1
A preparation process of a polytetrafluoroethylene film comprises the following steps:
(1) sieving raw materials: sieving the polytetrafluoroethylene resin DF-161 by a 10-mesh sieve for later use;
(2) compression molding: loading the sieved polytetrafluoroethylene resin DF-161 into a mold, boosting the pressure to 5MPa at the speed of 15mm/min at room temperature, withdrawing the press, boosting the pressure to 25MPa at the speed of 15mm/min again after 4-5 seconds, maintaining the pressure for 15min, and taking out for later use;
(3) and (3) sintering: putting the molded product obtained in the step (2) into a sintering furnace, heating from room temperature to 290 ℃ at the speed of 3 ℃/min, preserving heat at 290 ℃ for 10min, heating from 290 ℃ to 380 ℃ at the speed of 1 ℃/min, preserving heat at 380 ℃ for 8h, then cooling from 380 ℃ to 290 ℃ at the speed of 1 ℃/min, naturally cooling from 290 ℃ to room temperature, and taking out for later use;
(4) turning: and (4) insulating the sintered product obtained in the step (3) at 100 ℃ for 3h, and turning on a lathe to obtain the polytetrafluoroethylene film with the thickness of 0.5 mm.
Comparative example 2
A polytetrafluoroethylene film was prepared in example 4 of patent document CN 109203525A.
Comparative example 3
A process for preparing a polytetrafluoroethylene film, the steps being as described in example 1, except that: in the step (5), the pressurizing pressure is 0.05 MPa; the other steps were carried out in accordance with example 1 to obtain a polytetrafluoroethylene film having a thickness of 0.5 mm.
Comparative example 4
A process for preparing a polytetrafluoroethylene film, the steps being as described in example 1, except that: in the step (5), after the heating is stopped, naturally cooling to below 50 ℃ under the condition of continuously pressurizing to 0.3MPa, and finally taking out the film from the die to obtain a polytetrafluoroethylene film with the thickness of 0.5 mm; the other steps were in accordance with example 1.
Comparative example 5
A process for preparing a polytetrafluoroethylene film, the steps being as described in example 1, except that: the SSG of the polytetrafluoroethylene resin used in step (1) was 2.190. The other steps were carried out in accordance with example 1 to obtain a polytetrafluoroethylene film having a thickness of 0.5 mm.
Test examples
Testing the bending resistance of the polytetrafluoroethylene film prepared by the embodiment and the comparative example; the number of MIT flex endurance tests of the polytetrafluoroethylene film of the invention was measured according to GB/T2679.5-1995 MIT flex endurance test method, and the test results are shown in Table 1.
Table 1 examples and comparative performance test results
It can be seen from table 1 that the bending times of the embodiment of the present invention are greatly improved compared with the corresponding ratio, and the significant effects of the specific raw material polytetrafluoroethylene resin and the process of the present invention are fully verified.
Claims (3)
1. A preparation process of a bending-resistant polytetrafluoroethylene film comprises the following steps:
(1) sieving polytetrafluoroethylene resin powder by a 10-mesh screen, and then carrying out compression molding, sintering and turning to obtain a turned film;
the particle size of the polytetrafluoroethylene resin powder is 10-50 mu m; the polytetrafluoroethylene resin has a standard relative density (SSG) of 2.140 to 2.180; the compression molding comprises the following steps: increasing the pressure to 3-8MPa at the speed of 10-100mm/min at room temperature, returning the press, increasing the pressure to 10-50MPa at the speed of 10-100mm/min after 3-6 seconds, and maintaining the pressure for 3-30 min; the sintering conditions are as follows: heating from room temperature to 290 ℃ at the speed of 1-5 ℃/min, preserving heat at 290 ℃ for 5-15min, heating from 290 ℃ to 360-390 ℃ at the speed of 1-3 ℃/min, preserving heat for 6-10h, finally cooling to 290 ℃ at the speed of 1-3 ℃/min, and naturally cooling from 290 ℃ to room temperature; after sintering and before turning, the blank obtained by sintering needs to be insulated for 1-5h at 100 ℃;
(2) heating the turned film to be molten and pressurized, then stopping heating, and rapidly cooling to room temperature by using cold water under the condition of keeping the pressure unchanged to prepare the bending-resistant polytetrafluoroethylene film;
the heating temperature is controlled at 350-390 ℃, the heating is maintained for 5-15min after the melting, and the pressure of pressurization is controlled at 0.1-1 MPa; the temperature of the cold water is 0-20 ℃;
the obtained polytetrafluoroethylene film has the MIT bending-resistant times of more than 440 ten thousand.
2. The process for preparing a kink-resistant polytetrafluoroethylene film according to claim 1, characterized in that in step (1), the compression rate of said compression molding is 10-30mm/min, the pressure is 20-30MPa, and the dwell time is 10-20 min.
3. The process for preparing a kink-resistant ptfe film according to claim 1, wherein in step (2), the ptfe film has a thickness of 0.1 to 1.0 mm.
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