CN111574744A - Preparation method of clean environment-friendly polyvinylidene fluoride foamed sheet - Google Patents
Preparation method of clean environment-friendly polyvinylidene fluoride foamed sheet Download PDFInfo
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- CN111574744A CN111574744A CN202010440014.0A CN202010440014A CN111574744A CN 111574744 A CN111574744 A CN 111574744A CN 202010440014 A CN202010440014 A CN 202010440014A CN 111574744 A CN111574744 A CN 111574744A
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
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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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a preparation method of a clean environment-friendly polyvinylidene fluoride foamed sheet, which comprises the following steps: an extrusion step: firstly, adding polyvinylidene fluoride into a double-screw extruder to be extruded to form a polyvinylidene fluoride sheet; an irradiation step: carrying out electron beam irradiation crosslinking on the polyvinylidene fluoride sheet; and (3) gas saturation: putting the sheet into a heated high-pressure kettle, and injecting supercritical nitrogen into the high-pressure kettle to ensure that the irradiation cross-linked vinylidene fluoride sheet is completely saturated by the supercritical nitrogen; a nucleation step: decompressing and nucleating the irradiation crosslinked vinylidene fluoride sheet in an autoclave in the step of gas saturation, decompressing and opening the autoclave after the autoclave is cooled, and taking out the nucleated irradiation crosslinked vinylidene fluoride sheet; a foaming step: and after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, putting the nucleated irradiation crosslinked vinylidene fluoride sheet into the high-pressure kettle again for foaming, and taking out the nucleated irradiation crosslinked vinylidene fluoride sheet after foaming. According to the invention, supercritical nitrogen is used as a foaming agent, and the obtained foam sheet is clean and tasteless, uniform and fine in foam hole and excellent in mechanical property.
Description
Technical Field
The invention relates to the technical field of material forming, in particular to a preparation method of a polyvinylidene fluoride foamed sheet.
Background
The polymer foam material has the functions of light weight, heat insulation, sound insulation, buffering, shock absorption and the like, and is widely applied to the fields of traffic, buildings, packaging, daily necessities, sports equipment and the like. The high-performance foam material can also be used in the advanced fields of military, aerospace and the like. Currently, polystyrene foam (EPS), polyurethane foam (EPU), polyethylene foam (EPE), and the like are used as the foam material. The traditional foam materials have a plurality of defects in the aspects of heat resistance, chemical resistance, weather resistance, flame retardance and the like, and cannot meet the requirements of aerospace, microelectronic and semiconductor industries, petrochemical industries and pharmaceutical industries on the aspects of chemical resistance, flame retardance and the like of the foam materials.
The fluoropolymer has excellent characteristics such as heat resistance, chemical resistance, weather resistance, and flame retardancy. Belongs to a non-polluting raw material. These characteristics are mainly related to factors such as low polarizability of fluorine atoms in the fluoropolymer structure, strong electronegativity, small van der waals radius, high fluorocarbon bond energy, and the like. Due to the excellent characteristics of the fluorine-containing polymer, the fluorine-containing polymer is widely applied to various industries and fields such as national defense and military industry, aerospace, electronic and electric appliances, machinery, chemical engineering, textile, medicine and the like. Polyvinylidene fluoride (PVDF) is a new material with excellent comprehensive performance developed in the 70 s of the 20 th century, the annual growth rate is more than 10%, the yield accounts for about 14% of the total amount of all fluorine-containing plastics, and the PVDF is the second largest fluorine-containing resin with the annual yield only second to that of Polytetrafluoroethylene (PTFE). PVDF is a fluorine-containing resin prepared by homopolymerization or copolymerization of vinylidene fluoride monomers, and has the advantages of both fluorine-containing resin and common resin. The foam material with PVDF as the matrix has the excellent performances of both PVDF and foam materials, and can be used in many fields where the traditional foam materials can not meet the use conditions.
The PVDF foam sheets currently used in the market are mostly prepared by using a chemical foaming agent such as azodicarbonamide, and the chemical foaming agent can generate a substance, namely semicarbazide, which can cause cancers when being heated and decomposed, and the substance can enter foods and has the highest content in infant foods. The european union has therefore banned the sale and import of AC foaming agents as food packaging or as plastic materials and products in contact with food from 8/2 2005. The european union started to limit the amount of formamide in foamed products using AC as blowing agent in the end of 2010. This foaming technique limits the use of PVDF in many specific areas.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a supercritical nitrogen foamed polyvinylidene fluoride material.
In order to realize the purpose, the invention provides a preparation method of a clean environment-friendly polyvinylidene fluoride foamed sheet, which comprises the following steps:
extrusion step S1: firstly, adding polyvinylidene fluoride into a double-screw extruder to be extruded to form a polyvinylidene fluoride sheet;
irradiation step S2: carrying out electron beam irradiation crosslinking on the polyvinylidene fluoride sheet;
gas saturation step S3: putting the irradiation crosslinking vinylidene fluoride sheet into a heated high-pressure kettle, and injecting supercritical nitrogen into the high-pressure kettle by using a high-pressure pump to ensure that the irradiation crosslinking vinylidene fluoride sheet is completely saturated by the supercritical nitrogen;
nucleation step S4: decompressing the irradiation cross-linked vinylidene fluoride sheet in the high-pressure kettle of the gas saturation step S3 to make the irradiation cross-linked vinylidene fluoride sheet nucleate, decompressing and opening the kettle after the high-pressure kettle is cooled, and taking out the nucleated irradiation cross-linked vinylidene fluoride sheet;
foaming step S5: and after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, putting the nucleated irradiation crosslinked vinylidene fluoride sheet into the high-pressure kettle again for foaming, and taking out the nucleated irradiation crosslinked vinylidene fluoride sheet after foaming.
Preferably, the extrusion temperature in the extrusion step S1 is 150-210 ℃.
Preferably, the irradiation dose in the irradiation step S2 is 20 to 100 kGy.
Preferably, in the gas saturation step S3, the temperature of the autoclave is 180-220 ℃, after the irradiation-crosslinked vinylidene fluoride sheet is placed in the autoclave, the autoclave is purged with a small-flow supercritical nitrogen gas for 1-3min, then a high-pressure pump is used to inject a supercritical nitrogen gas into the autoclave, so that the pressure in the autoclave reaches 30-60MPa, and the constant temperature and pressure are maintained for 1-3 hours.
Preferably, in the gas saturation step S3, the saturation temperature of the irradiation-crosslinked vinylidene fluoride sheet fully saturated with supercritical nitrogen is 150-.
Preferably, in the nucleation step S4, before the autoclave is released from the autoclave, the autoclave is cooled to 30-70 ℃ after being kept at constant temperature and pressure for 1-3 hours, and then rapidly released from the autoclave to 30-60MPa in a short time by using a quick release valve to nucleate the irradiation crosslinked vinylidene fluoride sheet, and then the autoclave is cooled to 30-70 ℃ and released from the autoclave.
Preferably, in the nucleation step S4, the time for depressurizing the autoclave to 30 to 60MPa is controlled to 1 second by using a quick release valve.
Preferably, in the foaming step S5, after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, the nucleated irradiation crosslinked vinylidene fluoride sheet is placed into the autoclave again, the autoclave is pressurized to 2-5MPa, then the autoclave temperature is raised to the set temperature of 170-.
According to the preparation method of the clean environment-friendly polyvinylidene fluoride foamed sheet, irradiation crosslinking is performed on the polyvinylidene fluoride foamed sheet in an irradiation crosslinking mode, so that the melt strength of the polyvinylidene fluoride is improved, the completeness of foam holes in the foaming process is ensured, and the foam with a regular shape, stable size and good surface quality is obtained; the supercritical nitrogen is used as the foaming agent, the adopted foaming process is green and environment-friendly, and the obtained foam sheet is clean and tasteless, has uniform and fine foam holes and excellent mechanical property, and has great application value.
Drawings
FIG. 1 is a SEM image of example 1 of the cell structure of the clean and environment-friendly polyvinylidene fluoride foamed sheet prepared by the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a clean environment-friendly polyvinylidene fluoride foamed sheet, which comprises the following steps:
extrusion step S1: firstly, adding polyvinylidene fluoride into a double-screw extruder to be extruded to form a polyvinylidene fluoride sheet;
irradiation step S2: carrying out electron beam irradiation crosslinking on the polyvinylidene fluoride sheet;
gas saturation step S3: putting the irradiation crosslinking vinylidene fluoride sheet into a heated high-pressure kettle, and injecting supercritical nitrogen into the high-pressure kettle by using a high-pressure pump to ensure that the irradiation crosslinking vinylidene fluoride sheet is completely saturated by the supercritical nitrogen;
nucleation step S4: decompressing the irradiation cross-linked vinylidene fluoride sheet in the high-pressure kettle of the gas saturation step S3 to make the irradiation cross-linked vinylidene fluoride sheet nucleate, decompressing and opening the kettle after the high-pressure kettle is cooled, and taking out the nucleated irradiation cross-linked vinylidene fluoride sheet;
foaming step S5: and after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, putting the nucleated irradiation crosslinked vinylidene fluoride sheet into the high-pressure kettle again for foaming, and taking out the nucleated irradiation crosslinked vinylidene fluoride sheet after foaming.
Preferably, the extrusion temperature in the extrusion step S1 is 150-210 ℃.
Preferably, the irradiation dose in the irradiation step S2 is 20 to 100 kGy.
Preferably, in the gas saturation step S3, the temperature of the autoclave is 180-220 ℃, which can achieve the purpose of rapidly permeating supercritical nitrogen into the PVDF sheet, after the irradiation crosslinked vinylidene fluoride sheet is placed into the autoclave, the autoclave is purged with a small flow of supercritical nitrogen for 1-3min to displace the air in the autoclave to prevent the resin from oxidative degradation during the saturation process, and then the supercritical nitrogen is injected into the autoclave by a high pressure pump to make the pressure in the autoclave reach 30-60MPa, and the constant temperature and pressure are maintained for 1-3 hours, so that the saturation rate of the supercritical nitrogen can be increased under high pressure, and the sheet can be completely saturated for enough time.
Preferably, in the gas saturation step S3, the saturation temperature of the irradiation-crosslinked vinylidene fluoride sheet fully saturated with supercritical nitrogen is 150-.
Preferably, in the nucleation step S4, before the autoclave is released from the autoclave, the autoclave is cooled to 30-70 ℃ after being kept at constant temperature and pressure for 1-3 hours, and then rapidly released from the autoclave to 30-60MPa in a short time by using a quick release valve to nucleate the irradiation crosslinked vinylidene fluoride sheet, and then the autoclave is cooled to 30-70 ℃ and released from the autoclave. This prevents excessive expansion of the sheet during pressure relief opening of the kettle.
Preferably, in the nucleation step S4, the time for depressurizing the autoclave to 30-60MPa is controlled to be 1 second by using a quick release valve, so as to achieve quick nucleation and increase the cell density.
Preferably, in the foaming step S5, after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, the nucleated irradiation crosslinked vinylidene fluoride sheet is placed into the autoclave again, the autoclave is pressurized to 2-5MPa, then the autoclave temperature is raised to the set temperature of 170-.
According to the preparation conditions and parameters adopted in the examples 1 to 6 in the table 1, the clean and environment-friendly polyvinylidene fluoride foamed sheets are respectively produced according to the preparation method of the clean and environment-friendly polyvinylidene fluoride foamed sheets.
Table 1-preparation conditions, parameters and properties of examples 1 to 6
From the physical properties of the foams tested in examples 1 to 6 in table 1, the foam sheets prepared in the examples have good surface shape, regular shape, cleanness, no smell, uniform and fine cells and excellent mechanical properties. FIG. 1 is a SEM image of example 1 of the cell structure of the clean and environment-friendly polyvinylidene fluoride foamed sheet prepared by the method of the present invention. In addition, the sheet has low odor and good flame retardancy.
According to the preparation method of the clean environment-friendly polyvinylidene fluoride foamed sheet, irradiation crosslinking is performed on the polyvinylidene fluoride foamed sheet in an irradiation crosslinking mode, so that the melt strength of the polyvinylidene fluoride is improved, the completeness of foam holes in the foaming process is ensured, and the foam with a regular shape, stable size and good surface quality is obtained; the supercritical nitrogen is used as the foaming agent, the adopted foaming process is green and environment-friendly, and the obtained foam sheet is clean and tasteless, has uniform and fine foam holes and excellent mechanical property, and has great application value.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. The preparation method of the clean environment-friendly polyvinylidene fluoride foamed sheet is characterized by comprising the following steps:
extrusion step S1: firstly, adding polyvinylidene fluoride into a double-screw extruder to be extruded to form a polyvinylidene fluoride sheet;
irradiation step S2: carrying out electron beam irradiation crosslinking on the polyvinylidene fluoride sheet;
gas saturation step S3: putting the irradiation crosslinking vinylidene fluoride sheet into a heated high-pressure kettle, and injecting supercritical nitrogen into the high-pressure kettle by using a high-pressure pump to ensure that the irradiation crosslinking vinylidene fluoride sheet is completely saturated by the supercritical nitrogen;
nucleation step S4: decompressing the irradiation cross-linked vinylidene fluoride sheet in the high-pressure kettle of the gas saturation step S3 to make the irradiation cross-linked vinylidene fluoride sheet nucleate, decompressing and opening the kettle after the high-pressure kettle is cooled, and taking out the nucleated irradiation cross-linked vinylidene fluoride sheet;
foaming step S5: and after the nucleated irradiation crosslinked vinylidene fluoride sheet is cooled to room temperature, putting the nucleated irradiation crosslinked vinylidene fluoride sheet into the high-pressure kettle again for foaming, and taking out the nucleated irradiation crosslinked vinylidene fluoride sheet after foaming.
2. The method for preparing a clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein the extrusion temperature in the extrusion step S1 is 150-210 ℃.
3. The method for preparing a clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein the irradiation dose in the irradiation step S2 is 20-100 kGy.
4. The method for preparing a clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein in the gas saturation step S3, the temperature of the autoclave is 180-.
5. The method for preparing a clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein in the gas saturation step S3, the saturation temperature of the irradiation crosslinked polyvinylidene fluoride sheet fully saturated with supercritical nitrogen is 150-200 ℃, and the saturation pressure is 30-60 MPa.
6. The method for preparing clean and environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein in the nucleation step S4, before the autoclave is opened by pressure release, the autoclave is rapidly released to 30-60MPa by a quick release valve in a short time after the autoclave is cooled to 30-70 ℃ for 1-3 hours at constant temperature and pressure, so as to nucleate the irradiation crosslinked polyvinylidene fluoride sheet, and then the autoclave is cooled to 30-70 ℃ and then released to open the autoclave.
7. The method for preparing clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 6, wherein in the nucleation step S4, the time for depressurizing the autoclave to 30-60MPa is controlled to be 1 second by using a quick release valve.
8. The method for preparing clean environment-friendly polyvinylidene fluoride foamed sheet according to claim 1, wherein in the foaming step S5, the cross-linked polyvinylidene fluoride sheet is placed in an autoclave again after being cooled to room temperature by nucleation irradiation, the autoclave is pressurized to 2-5MPa, then the autoclave is heated to a set temperature of 170-200 ℃, and the autoclave is discharged to normal pressure for foaming by using a fine adjustment valve after heat preservation and pressure maintenance for 10-30 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112592549A (en) * | 2020-11-23 | 2021-04-02 | 深圳市长园特发科技有限公司 | Radiation crosslinking polyvinylidene fluoride foam material and preparation method thereof |
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| US20100249255A1 (en) * | 2007-11-12 | 2010-09-30 | Zotefoams Plc | Fluoropolymer foams prepared with the use of blowing agents and applications thereof |
| CN106146874A (en) * | 2016-06-01 | 2016-11-23 | 湖州长园特发科技有限公司 | A kind of supercritical fluid expanded polyolefin material and preparation method thereof |
| CN109081936A (en) * | 2017-06-14 | 2018-12-25 | 宁波绿色方舟环境科技有限公司 | A kind of fluoropolymer cellular material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100249255A1 (en) * | 2007-11-12 | 2010-09-30 | Zotefoams Plc | Fluoropolymer foams prepared with the use of blowing agents and applications thereof |
| CN106146874A (en) * | 2016-06-01 | 2016-11-23 | 湖州长园特发科技有限公司 | A kind of supercritical fluid expanded polyolefin material and preparation method thereof |
| CN109081936A (en) * | 2017-06-14 | 2018-12-25 | 宁波绿色方舟环境科技有限公司 | A kind of fluoropolymer cellular material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112592549A (en) * | 2020-11-23 | 2021-04-02 | 深圳市长园特发科技有限公司 | Radiation crosslinking polyvinylidene fluoride foam material and preparation method thereof |
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