CN101704308B - Preparation method of polyolefin three-layer composite microporous membrane - Google Patents
Preparation method of polyolefin three-layer composite microporous membrane Download PDFInfo
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- CN101704308B CN101704308B CN200910075830XA CN200910075830A CN101704308B CN 101704308 B CN101704308 B CN 101704308B CN 200910075830X A CN200910075830X A CN 200910075830XA CN 200910075830 A CN200910075830 A CN 200910075830A CN 101704308 B CN101704308 B CN 101704308B
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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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92923—Calibration, after-treatment or cooling zone
Abstract
A polyolefin three-layer composite microporous membrane and a preparation method thereof are disclosed, aiming at solving the problems of difficult technique control and non-uniform product pores. Raw materials polyethylene and polypropylene are prepared into polypropylene/polyethylene/polypropylene three-layer composite microporous membrane, wherein an adhesive substance is added into the raw material polyethylene; the technique comprises the following steps: a. curtain coating preparation of basement-membrane; b. multistage annealing treatment; c. three-layer basement-membrane composition; d. multipoint stretching pore-forming; and e. thermoforming treatment. The invention has the advantages of undamaged basement-membrane, good safety, simple preparation, small equipment investment, non-blockage of membrane pores during preparation process, high porosity, easy control of porosity and the like, is suitable for making polyolefin microporous membrane of various types used for breathability material, ultrafiltration, membrane filtration, super capacitor and battery diaphragm materials, etc.
Description
Technical field
The present invention relates to a kind of preparation method of polyolefin compound microporous membrane.
Background technology
Along with development and the extensive use of lithium ion battery product, also more and more higher to the specification requirement of the used polyphosphazene polymer alkene of battery diaphragm material MULTILAYER COMPOSITE microporous barrier.In known technology, existing polyolefin multi-layer composite micro porous film mainly is three layers of compound microporous barrier of polypropylene, polyethylene/polypropylene, its preparation method has by blowing being extruded the polypropylene that obtains, polyethylene atresia basement membrane, then the mode of pressing is compound by centering m-polyethylene layer hot melt, and then polypropylene, polyethylene/polypropylene three-layer composite microporous membrane is made in the also simple tension of annealing, but the complex method of hot melt pressing will be first with the polyethylene based film melting, therefore physical property and the lamellar structure of polyethylene based film are produced destruction, cause rupture of membranes in the drawing process, the unequal phenomenon of product hole.The combination process that also has adopts multi-layer co-extruded mode, it forms polyolefin three-layer or MULTILAYER COMPOSITE basement membrane with polyethylene and pp material by two or more extruders and co-extrusion die head blowing or curtain coating, and polyolefin three-layer or MULTILAYER COMPOSITE microporous barrier are made in annealed and stretching again.But adopt this kind complex method, because polypropylene and polyethylene annealing process require to differ greatly, cause technique controlling difficulty large, and the equipment formation is complicated, equipment investment is larger, and is also higher to the specification requirement of equipment.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and do not destroy basement membrane, security performance is good, simple to operate, manufacturing process is not stopped up fenestra, porosity is high and porosity is held manageable polyolefin three-layer composite microporous membrane and preparation method thereof.
Addressing the above problem the technical scheme that adopts is:
A kind of polyolefin three-layer composite microporous membrane, it makes polypropylene, polyethylene/polypropylene three-layer composite microporous membrane take polyethylene and polypropylene as raw material, wherein adds stickum in the polyethylene raw material; Described stickum is one or more in the random copolymer of ethene, vinyl acetate, acrylate copolymer and ethene and acrylate; The mass percent addition of described caking property material is 0.01～7.00% of polyethylene quality.
A kind of method for preparing polyolefin three-layer composite microporous membrane, its preparation section step is as follows:
A. basement membrane preparation, with raw material polypropylene and the polyethylene that contains caking property material heating and melting respectively, wherein, polypropylene is 190～270 ℃, polyethylene is 160～270 ℃; Extrude by T-shaped casting head, it is 0.5～5.0mm that the die orifice of die head is opened gap, and draft speed is 50～200 m/mins, makes basement membrane;
B. annealing in process is put into baking oven with the basement membrane of making among the step a and is carried out annealing in process, and oven temperature is 70～155 ℃, and annealing time is 10 minutes～24 hours, after annealing, its degree of crystallinity is reached more than 60%, forms laterally regularly arranged platelet;
C. three layers of basement membrane are compound, caking property material after the annealing in the polyethylene moves to the surface, two layers of polypropylene basement membrane therebetween among the step b is connected polyethylene based film, the compound three layers of compound atresia basement membrane of polypropylene, polyethylene/polypropylene of making, under 80～120 ℃ of conditions, constant temperature 1～30 minute is realized solidifying;
D. hole forming by multipoint stretching, three layers of compound atresia basement membrane of polypropylene, polyethylene/polypropylene of making among the step c are stretched under 10～155 ℃, drafting rate is 0.1～30.0 m/min, draw ratio is 100%～400%, first 10～100 ℃ temperature and 300～900%/minute stretching ratio under carry out cold drawn formation crazing defective, and then 100～155 ℃ temperature and 100～400%/minute stretching ratio under further stretch and form microcellular structure;
E. thermal finalization is processed, the laminated film that forms micropore after stretching in the steps d is carried out first negative stretch, promote the elimination of internal stress, thermal finalization was processed 5 minutes～10 hours under 60～160 ℃ of conditions again, namely became polypropylene, polyethylene/polypropylene three-layer composite microporous membrane.
The preparation method of said polyolefins three-layer composite microporous membrane, the annealing process of described annealing in process step b is divided into 2～6 sections, namely according to the oven temperature of setting from low to high, be divided into 2～6 thermograde sections and finish annealing operation.
The preparation method of said polyolefins three-layer composite microporous membrane adopts 3～40 drawing points in the described hole forming by multipoint stretching step.
The preparation method of said polyolefins three-layer composite microporous membrane, negative stretch in the described thermal finalization treatment step refers to the single thin film behind the stretching pore-forming is stretched under 90～155 ℃ temperature conditions, its draw ratio is negative value, concrete operation method is that the linear velocity of film is slowed down according to certain ratio at draw direction, makes the microporous barrier after the stretching produce stress relaxation.
The present invention prepares basement membrane with raw material polypropylene and polyethylene according to above-mentioned processing step a. curtain coating; B. multi-stage annealing processing; C. three layers of basement membrane are compound; D. hole forming by multipoint stretching and e. thermal finalization are processed this 5 step and namely be can be made into the polyolefin three-layer composite microporous membrane product.
Adopt technique scheme, the present invention to solve effectively that technique controlling difficulty in the existing polyolefin three-layer composite microporous membrane preparation method is large, the problem of product hole inequality.Show through test of many times, compared with prior art, it has does not destroy basement membrane, and security performance is good, makings is simple, and equipment investment is little, and manufacturing process is not stopped up fenestra, and porosity is high, and the advantage such as the easy control of porosity.Stickum in the described polyethylene has to the characteristic of film surface migration, the blockage of the micro orifice problem of having avoided thus surperficial coated with adhesive to bring.Be suitable for making used various types of MIcroporous polyolefin films such as poromeric material, ultrafiltration, membrane filtration, ultracapacitor and battery diaphragm material.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Open gap 1.2mm by extruder at the die orifice of T-shaped casting head after pp material is heated to 240 ℃ of meltings, chill-roll temperature is 30 ℃, extrudes under 180 m/mins of conditions of drafting rate and makes basement membrane; The mixture of polyethylene and ethylene-acrylate random copolymer melt extrudes at casting machine under 200 ℃, and the consumption of ethylene-acrylate random copolymer is 1.2%, and die orifice is opened gap 1.2mm, 25 ℃ of chill-roll temperature, 150 m/mins of drafting rates.The basement membrane annealing in process, 150 ℃ of polypropylene annealing temperatures, annealing time 15 minutes, 80 ℃ of polyethylene based film annealing temperatures, annealing time 2 hours.Carry out according to polypropylene, polyethylene/polyacrylic order compound, 80 ℃ of lower constant temperature 20 minutes.Simple tension, draw ratio are 350%, and typing is 10 minutes after stretching, and makes a kind of polypropylene, polyethylene/polypropylene three-layer composite microporous membrane product, and its performance sees the following form 1.
Embodiment 2
Open gap 1.2mm by extruder at the die orifice of T-shaped casting head after pp material is heated to 240 ℃ of meltings, chill-roll temperature is 30 ℃, extrudes under 180 m/mins of conditions of drafting rate and makes basement membrane; The mixture of polyethylene and ethylene-acrylate random copolymer melt extrudes at casting machine under 200 ℃, and the consumption of ethylene-acrylate random copolymer is 1.2%, and die orifice is opened gap 1.2mm, 25 ℃ of chill-roll temperature, 150 m/mins of drafting rates.Basement membrane annealing in process, polypropylene annealing temperature are respectively 90 ℃, 105 ℃ and 120 ℃ (time correspond to respectively 30 minutes, 30 minutes and 60 minutes), and polyethylene is respectively 80 ℃ and 100 ℃ (time corresponds to respectively 1 hour and 30 minutes).Carry out according to polypropylene, polyethylene/polyacrylic order compound, 100 ℃ of lower constant temperature 20 minutes.Simple tension, draw ratio 350%, typing is 10 minutes after stretching, and makes a kind of polyolefin three-layer composite microporous membrane product, and its performance sees the following form 1.
Embodiment 3
Open gap 1.2mm by extruder at the die orifice of T-shaped casting head after pp material is heated to 240 ℃ of meltings, 30 ℃ of chill-roll temperature are extruded under 180 m/mins of conditions of drafting rate and are made basement membrane; The mixture of polyethylene and ethylene-acrylate random copolymer melt extrudes at casting machine under 200 ℃, and the consumption of ethylene-acrylate random copolymer is 0.8%, and die orifice is opened gap 1.2mm, and chill-roll temperature is 25 ℃, 150 m/mins of drafting rates.Basement membrane annealing in process, polypropylene annealing temperature are respectively 90 ℃, 100 ℃ and 120 ℃ (annealing respectively 30 minutes), and polyethylene is respectively 90 ℃ and 105 ℃ (annealing respectively 60 minutes).Carry out according to polypropylene, polyethylene/polyacrylic order compound, 100 ℃ of lower constant temperature 20 minutes.Simple tension, draw ratio are 350%, and typing is 8 minutes after stretching, and makes a kind of polypropylene, polyethylene/polypropylene three-layer composite microporous membrane product, and its performance sees the following form 1.
Table 1 microporous barrier performance comparison table
Porosity among the present invention adopts mercury injection apparatus to measure; Gas permeability adopts Gurley air permeability measuring instrument to measure; Peel strength adopts draws a compression test measurement, and detachment rate is 6 inch per minute clocks.
Claims (4)
1. the method for a polyolefin three-layer composite microporous membrane is characterized in that, it makes polypropylene, polyethylene/polypropylene three-layer composite microporous membrane take polyethylene and polypropylene as raw material, wherein adds stickum in the polyethylene raw material; Described stickum is one or more in the random copolymer of ethene, vinyl acetate, acrylate copolymer and ethene and acrylate; The mass percent addition of described caking property material is 0.01～7.00% of polyethylene quality;
The preparation section step is as follows:
A. basement membrane preparation, with raw material polypropylene and the polyethylene that contains caking property material heating and melting respectively, wherein, polypropylene is 190～270 ℃, polyethylene is 160～270 ℃; Extrude by T-shaped casting head, it is 0.5～5.0mm that the die orifice of die head is opened gap, and draft speed is 50～200 m/mins, makes basement membrane;
B. annealing in process is put into baking oven with the basement membrane of making among the step a and is carried out annealing in process, and oven temperature is 70～155 ℃, and annealing time is 10 minutes～24 hours, after annealing, its degree of crystallinity is reached more than 60%, forms laterally regularly arranged platelet;
C. three layers of basement membrane are compound, caking property material after the annealing in the polyethylene moves to the surface, two layers of polypropylene basement membrane therebetween among the step b is connected polyethylene based film, the compound three layers of compound atresia basement membrane of polypropylene, polyethylene/polypropylene of making, under 80～120 ℃ of conditions, constant temperature 1～30 minute is realized solidifying;
D. hole forming by multipoint stretching, three layers of compound atresia basement membrane of polypropylene, polyethylene/polypropylene of making among the step c are stretched under 10～155 ℃, drafting rate is 0.1～30.0 m/min, draw ratio is 100%～400%, first 10～100 ℃ temperature and 300～900%/minute stretching ratio under carry out cold drawn formation crazing defective, and then 100～155 ℃ temperature and 100～400%/minute stretching ratio under further stretch and form microcellular structure;
E. thermal finalization is processed, the laminated film that forms micropore after stretching in the steps d is carried out first negative stretch, promote the elimination of internal stress, thermal finalization was processed 5 minutes～10 hours under 60～160 ℃ of conditions again, namely became polypropylene, polyethylene/polypropylene three-layer composite microporous membrane.
2. the preparation method of described polyolefin three-layer composite microporous membrane according to claim 1, it is characterized in that, the annealing process of described annealing in process step b is divided into 2～6 sections, namely according to the oven temperature of setting from low to high, be divided into 2～6 thermograde sections and finish annealing operation.
3. the preparation method of described polyolefin three-layer composite microporous membrane according to claim 2 is characterized in that, adopts 3～40 drawing points in the described hole forming by multipoint stretching step.
4. the preparation method of described polyolefin three-layer composite microporous membrane according to claim 3, it is characterized in that, negative stretch in the described thermal finalization treatment step refers to the single thin film behind the stretching pore-forming is stretched under 90～155 ℃ temperature conditions, its draw ratio is negative value, during operation the linear velocity of film is slowed down according to certain ratio at draw direction, make the microporous barrier after the stretching produce stress relaxation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102729532B (en) * | 2012-06-11 | 2015-07-01 | 达尼特材料科技（芜湖）有限公司 | Multilayer porous membrane and preparation method thereof |
| CN102881852A (en) * | 2012-09-28 | 2013-01-16 | 达尼特材料科技（芜湖）有限公司 | Method and device for manufacturing microporous films |
| CN102956859B (en) * | 2012-11-28 | 2015-11-18 | 广东工业大学 | A kind of preparation method of multi-layer polyolefin composite micro porous film |
| CN103273654B (en) * | 2013-04-24 | 2015-11-25 | 深圳中兴创新材料技术有限公司 | The MIcroporous polyolefin film of a kind of ultra-thin method for preparing polyolefin microporous membrane and preparation thereof |
| CN103647036B (en) * | 2013-12-10 | 2016-01-06 | 深圳市星源材质科技股份有限公司 | A kind of preparation method of high strength microporous lithium ion battery separator and battery diaphragm |
| US10569230B2 (en) | 2015-05-30 | 2020-02-25 | Core Energy Recovery Solutions Inc. | Supported water vapor transport membrane comprising polyethylene oxide copolymer |
| CN105252793B (en) * | 2015-09-07 | 2017-07-25 | 浙江中财管道科技股份有限公司 | A kind of atactic copolymerized polypropene (PP R) tubing annealing process |
| CN108281593B (en) * | 2017-12-29 | 2022-01-25 | 武汉中兴创新材料技术有限公司 | Method for preparing polypropylene/polyethylene/polypropylene three-layer composite microporous membrane |
| CN109130443A (en) * | 2018-09-02 | 2019-01-04 | 佛山鹏程易胜机械有限公司 | A kind of dry method diaphragm stretching production line |
| CN110406137A (en) * | 2019-06-26 | 2019-11-05 | 佛山市盈博莱科技股份有限公司 | A kind of preparation method of high porosity polyolefin diaphragm of lithium ion battery |
| CN114347518B (en) * | 2021-12-31 | 2023-06-02 | 漳州杰安塑料有限公司 | PLA straw crystallization process |
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2009
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| US5013439A (en) * | 1988-05-12 | 1991-05-07 | Hoechst Celanese Corporation | Microporous membranes having increased pore densities and process for making the same |
| CN1504498A (en) * | 2002-12-03 | 2004-06-16 | 李春香 | Polyolefine multiple micoporous film and preparing process thereof |
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| CN101291794A (en) * | 2005-10-19 | 2008-10-22 | 东燃化学株式会社 | Process for producing multilayered microporous polyolefin film |
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