CN101695869A - Preparation method of polyolefin microporous film - Google Patents
Preparation method of polyolefin microporous film Download PDFInfo
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- CN101695869A CN101695869A CN200910075831A CN200910075831A CN101695869A CN 101695869 A CN101695869 A CN 101695869A CN 200910075831 A CN200910075831 A CN 200910075831A CN 200910075831 A CN200910075831 A CN 200910075831A CN 101695869 A CN101695869 A CN 101695869A
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Abstract
The invention relates to a preparation method of a polyolefin microporous film, aiming to solve the problems that the traditional preparation method of the polyolefin microporous film has complicated process, low production speed and poorer uniformity of microporous space. A polyolefin microporous film product is prepared by the following steps: a. base film preparation by casting; b. multi-stage annealing processing; c. hole forming by multipoint stretching; and d. heat setting processing. The method does not need solvent, has no pollution to the environment, low equipment investment, high production speed and uniform microporous space, and is suitable for preparing various polyolefin microporous films used for poromeric materials, ultra filtration, film filtration, super capacitors, battery diaphragm materials and the like.
Description
Technical field
The present invention relates to a kind of preparation method of MIcroporous polyolefin film.
Background technology
MIcroporous polyolefin film is a polymeric membrane, be the perforated membrane of aperture between 5nm～1000nm, the individual layer MIcroporous polyolefin film is applied to poromeric material such as diaper, medical dressing, clothes lining, fluid separation applications, ultrafiltration and membrane filtration, and in ultracapacitor and the battery diaphragm material.Along with the growing and extensive use of macromolecule product, also more and more higher to the specification requirement of the used macromolecule MIcroporous polyolefin film of macromolecule product especially poromeric material, ultrafiltration, membrane filtration, ultracapacitor and battery diaphragm material.In known technology, existing method for preparing polyolefin microporous membrane mainly contains two kinds of dry method (fusion drawn method) and wet methods (thermally induced phase separation), and wherein dry method specifically is divided into simple tension method and biaxial tension method again.Wet processing is to add in polyolefin as pore-foaming agent the higher boiling small-molecule substance and be dissolved in organic solvent to form the casting sheet, and cooling is separated then, takes out little molecule with organic solvent extracting, carries out forming microcellular structure after the biaxial tension.Need a large amount of solvents in the wet method preparation process, usually cause environmental pollution, and the technology relative complex, equipment investment is bigger.The dry method stretch processes mainly is by add the beta crystal improver with nucleation in polypropylene, the transformation of β crystal orientation α crystalline substance takes place in drawing process, utilize the difference of density between the different phases of polypropylene to form microcellular structure, be used to produce individual layer PP microporous barrier.But, cause microporous barrier porous nickel degree relatively poor, and this technology is higher to the specification requirement of production equipment because the minimum difficulty conversion ratio big, β crystal orientation α crystalline substance that mixes of the addition of beta crystal improver is wayward.Dry method simple tension technology is the method for producing the hard elastics sheet by melt extruding, and prepares the polyolefin base membrane of low-crystallinity, high orientation, carries out the film that high annealing obtains high-crystallinity then in baking oven; Again this film is formed microporous barrier through two step simple tensions, the first step is stretched at low temperatures crazing defective earlier, and second step stretched the crazing defective to amplify and forms microcellular structure; Existing dry method simple tension technology all adopts under the single temperature and anneals, and drawing point is less, causes microporous barrier distribution of pores homogeneity relatively poor, and throughput rate is lower.The simple tension technology that also has has added one-component nucleator and vegetable oil when the preparation microporous polypropylene membrane, complex process, and formed microporous barrier porous nickel degree is relatively poor.So far, can high-speed production (reaching more than 20 meters/minute) the hole homogeneity preferably the production technology of MIcroporous polyolefin film yet there are no report.
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, solve existing complicated process of preparation, throughput rate is low, microporous barrier hole homogeneity is relatively poor problem, provide a kind of free from environmental pollution, equipment investment is little, throughput rate is high, the method for preparing polyolefin microporous membrane of micropore porous nickel.
Addressing the above problem the technical scheme that is adopted is:
A kind of method for preparing polyolefin microporous membrane, it is undertaken by following operation:
A, curtain coating prepare basement membrane, or/and any in the polyethylene raw material is 190～270 ℃ at polypropylene, polyethylene is under 160～270 ℃ the condition, raw material to be carried out fusion with the raw material polypropylene, adopts The tape casting to make basement membrane;
B, annealing in process go into the basement membrane for preparing in the steps A to carry out annealing in process in the baking oven, and oven temperature is 70～155 ℃, for time of monofilm annealing in process be 10 minutes～24 hours;
C, hole forming by multipoint stretching, basement membrane after the annealing in process among the step B is stretched down at 10～155 ℃, drafting rate is 0.1～30.0 meter/minute, draw ratio is 100%～400%, earlier 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;
D, thermal finalization are handled, the film that the back that stretches among the step C is formed micropore carries out negative stretch earlier, eliminates the part internal stress, again with microporous polypropylene membrane at 70～160 ℃, polyethene microporous membrane thermal finalization under 60～130 ℃ of conditions was handled 5 minutes～10 hours, promptly became the MIcroporous polyolefin film product.
Said polyolefins microporous barrier preparation method, the annealing process of described annealing in process step B is divided into 2～6 sections, promptly according to the oven temperature of setting from low to high, be divided into 2～6 thermograde sections and finish annealing operation.
Said polyolefins microporous barrier preparation method, described hole forming by multipoint stretching step C adopt 3～40 drawing points.
Said polyolefins microporous barrier preparation method, negative stretch among the described thermal finalization treatment step D is meant the single thin film behind the stretching pore-forming is stretched under 90～155 ℃ temperature conditions, its draw ratio is a 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.
Said polyolefins microporous barrier preparation method, described raw material is polyethylene and polyacrylic mixture, its technology is identical with the making step of polyethene microporous membrane.
The present invention prepares basement membrane with material polyethylene or polypropylene or polyethylene and polypropylene miser according to above-mentioned A, curtain coating; B, multi-stage annealing processing; C, hole forming by multipoint stretching; D, thermal finalization are handled these 4 process and are made, and make the MIcroporous polyolefin film product.
Because the present invention designs and adopted technique scheme, has solved existing method for preparing polyolefin microporous membrane complex process effectively, throughput rate is less, the relatively poor problem of formed microporous barrier porous nickel degree.Show through testing result on trial for several times, it compared with prior art, has the manufacture craft novelty, design innovation does not need solvent, and is free from environmental pollution, equipment investment is little, the throughput rate height, advantages such as the microporous barrier porous nickel that forms are suitable for making and are used for used various 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:
With the polypropylene is raw material, and its index is a mean molecule quantity 300000, density 0.902g/cm
3, melt index 3.0 grams/10 minutes.Concrete operation is:
A1, curtain coating prepare basement membrane, under 240 ℃ condition, adopt T type curtain coating head to melt extrude the raw material polypropylene, and die orifice is opened crack 1.2mm, and chill-roll temperature is 30 ℃, and 180 meters/minute of drafting rates are made basement membrane;
B1, annealing in process go into the basement membrane of preparation in the steps A 1 to carry out annealing in process in the baking oven, and oven temperature is 150 ℃, for time of monofilm annealing in process be 15 minutes;
C1, hole forming by multipoint stretching, basement membrane after the annealing in process among the step B1 is carried out earlier cold drawn formation crazing defective under 20 ℃ and 350%/minutes stretching ratio, and then 145 ℃ temperature and 150%/minute stretching ratio under carry out the multiple spot formation microcellular structure that stretches;
D1, thermal finalization are handled, and the film that the back that stretches among the step C1 is formed micropore carries out negative stretch earlier, and it is 3% that speed reduces ratio, microporous polypropylene membrane thermal finalization under 110 ℃ of conditions are handled 12 minutes again, promptly become the microporous polypropylene membrane product.
Embodiment 2:
With the polyethylene is raw material, and its index is a mean molecule quantity 200000, and density is 0.964g/cm
3,/10 minutes high density polyethylene of melt index 0.4 gram.Concrete operation is:
A2, curtain coating prepare basement membrane, under 200 ℃ condition, adopt T type curtain coating head to melt extrude material polyethylene, and die orifice is opened crack 1.2mm, and chill-roll temperature is 25 ℃, and 180 meters/minute of drafting rates are made basement membrane;
B2, annealing in process go into the basement membrane for preparing in the steps A to carry out annealing in process in the baking oven, and oven temperature is 90 ℃, for time of monofilm annealing in process be 2 hours;
C2, hole forming by multipoint stretching, basement membrane after the annealing in process among the step B is carried out earlier cold drawn formation crazing defective under 28 ℃ and 400%/minutes stretching ratio, and then 105 ℃ temperature and 150%/minute stretching ratio under carry out the multiple spot formation microcellular structure that stretches;
D2, thermal finalization are handled, and the film that the back that stretches among the step C is formed micropore carries out negative stretch earlier, and it is 3% that speed reduces ratio, polyethene microporous membrane thermal finalization under 115 ℃ of conditions are handled 10 minutes again, promptly become the polyethene microporous membrane product.
Embodiment 3:
With the polypropylene is raw material, and its index is a mean molecule quantity 300000, and density is 0.902g/cm
3, melt index 3.0 grams/10 minutes.
Concrete operation is:
A3, curtain coating prepare basement membrane, and the raw material polypropylene under 230 ℃ condition, is melt extruded on casting machine, and die orifice is opened crack 1.2mm, and chill-roll temperature is 30 ℃, and 180 meters/minute of drafting rates are made basement membrane;
B3, annealing in process go into the basement membrane of preparation in the steps A 1 to carry out annealing in process in the baking oven, all anneal 30 minutes under 90 ℃, 105 ℃, 120 ℃ conditions respectively;
C3, hole forming by multipoint stretching, basement membrane after the annealing in process among the step B1 is formerly carried out cold drawn formation crazing defective under 23 ℃ and 400%/minutes stretching ratio, and then 140 ℃ temperature and 150%/minute stretching ratio under carry out multiple spot and stretch and form microcellular structure;
D3, thermal finalization are handled, and the film that the back that stretches among the step C1 is formed micropore carries out negative stretch earlier, and it is 4% that speed reduces ratio, microporous polypropylene membrane thermal finalization under 100 ℃ of conditions are handled 8 minutes again, promptly become the microporous polypropylene membrane product.
Microporous barrier performance indications such as following table among the embodiment 1-3:
Porosity among the present invention adopts mercury injection apparatus to measure; Gas permeability adopts Gurley air permeability measuring instrument to measure.
Claims (4)
1. a method for preparing polyolefin microporous membrane is characterized in that, it is undertaken by following operation:
A, curtain coating prepare basement membrane, or/and any in the polyethylene raw material is 190～270 ℃ at polypropylene, polyethylene is under 160～270 ℃ the condition, raw material to be carried out fusion with the raw material polypropylene, adopts The tape casting to make basement membrane;
B, annealing in process go into the basement membrane for preparing in the steps A to carry out annealing in process in the baking oven, and oven temperature is 70～155 ℃, for the monofilm annealing in process time be 10 minutes～24 hours;
C, hole forming by multipoint stretching stretch the basement membrane after the annealing in process among the step B down at 10～155 ℃, and drafting rate is 0.1～30.0 meter/minute, and draw ratio is 100%～400%; At 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;
D, thermal finalization are handled, the film that the back that stretches among the step C is formed micropore carries out negative stretch earlier, eliminates the part internal stress, again with microporous polypropylene membrane at 70～160 ℃, polyethene microporous membrane thermal finalization under 60～130 ℃ of conditions was handled 5 minutes～10 hours, promptly became the MIcroporous polyolefin film product.
2. method for preparing polyolefin microporous membrane according to claim 1 is characterized in that, the annealing process of described annealing in process process B is divided into 2～6 sections, promptly according to the oven temperature of setting from low to high, be divided into 2～6 thermograde sections and finish annealing operation.
3. method for preparing polyolefin microporous membrane according to claim 2 is characterized in that, described hole forming by multipoint stretching operation C adopts 3～40 drawing points.
4. method for preparing polyolefin microporous membrane according to claim 3 is characterized in that, the negative stretch among the described thermal finalization treatment step D is meant the single thin film behind the stretching pore-forming is stretched that its draw ratio is a negative value under 90～155 ℃ temperature conditions.
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Cited By (20)
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| CN102001186A (en) * | 2010-10-13 | 2011-04-06 | 深圳市星源材质科技股份有限公司 | Method for forming polyolefin microporous membrane and application thereof |
| WO2012062011A1 (en) * | 2010-11-12 | 2012-05-18 | 深圳市星源材质科技股份有限公司 | Method for preparing microporous polyolefin membrane and application thereof |
| CN102544414A (en) * | 2012-02-16 | 2012-07-04 | 南通天丰电子新材料有限公司 | Preparation method of high-temperature-resistant safe diaphragm |
| CN102683632A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Unilateral stretching method for inducing and producing safety diaphragm with microporous structure |
| CN102683631A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Two-way synchronous stretching method for manufacturing high temperature resistant diaphragm with uniform and adjustable microporous structure |
| CN102683630A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Two-way synchronous stretching method for inducing and producing safety diaphragm with microporous structure |
| 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 |
| CN102922849A (en) * | 2012-11-08 | 2013-02-13 | 温州市金田塑业有限公司 | Biaxially-oriented polypropylene (BOPP) ventilated water-blocking membrane and preparation method thereof |
| CN103205871A (en) * | 2013-04-27 | 2013-07-17 | 中材科技股份有限公司 | Regularization technology of reticular membrane |
| CN103273654A (en) * | 2013-04-24 | 2013-09-04 | 深圳中兴创新材料技术有限公司 | Preparation method for ultrathin polyolefin microporous membrane, and polyolefin microporous membrane prepared by same |
| CN103633272A (en) * | 2013-12-10 | 2014-03-12 | 深圳市星源材质科技有限公司 | Preparation method for microporous diaphragm and microporous diaphragm |
| CN103978705A (en) * | 2014-05-23 | 2014-08-13 | 四川大学 | Annealing method of polypropylene microporous membrane |
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| CN105489813A (en) * | 2015-11-03 | 2016-04-13 | 深圳市星源材质科技股份有限公司 | Thermal treatment method for lithium battery diaphragm through dry method |
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| CN102683630B (en) * | 2012-04-27 | 2015-05-20 | 范建国 | Two-way synchronous stretching method for inducing and producing safety diaphragm with microporous structure |
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| CN102683631A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Two-way synchronous stretching method for manufacturing high temperature resistant diaphragm with uniform and adjustable microporous structure |
| CN102683630A (en) * | 2012-04-27 | 2012-09-19 | 南通天丰电子新材料有限公司 | Two-way synchronous stretching method for inducing and producing safety diaphragm with microporous structure |
| CN102683632B (en) * | 2012-04-27 | 2015-08-12 | 范建国 | The method of producing microcellular structure blowout disk is brought out in simple tension |
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| 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 |
| CN102922849A (en) * | 2012-11-08 | 2013-02-13 | 温州市金田塑业有限公司 | Biaxially-oriented polypropylene (BOPP) ventilated water-blocking membrane and preparation method thereof |
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| CN103978705A (en) * | 2014-05-23 | 2014-08-13 | 四川大学 | Annealing method of polypropylene microporous membrane |
| CN104175544A (en) * | 2014-08-26 | 2014-12-03 | 天津大学 | Preparation method of microporous polypropylene film |
| US10569230B2 (en) | 2015-05-30 | 2020-02-25 | Core Energy Recovery Solutions Inc. | Supported water vapor transport membrane comprising polyethylene oxide copolymer |
| CN105489813A (en) * | 2015-11-03 | 2016-04-13 | 深圳市星源材质科技股份有限公司 | Thermal treatment method for lithium battery diaphragm through dry method |
| CN105489813B (en) * | 2015-11-03 | 2018-08-03 | 深圳市星源材质科技股份有限公司 | A kind of heat treatment method for dry method lithium electric separator |
| CN105500724A (en) * | 2015-12-18 | 2016-04-20 | 江苏安瑞达新材料有限公司 | Preparation method of separators of lithium power batteries |
| CN111098533A (en) * | 2019-12-31 | 2020-05-05 | 武汉中兴创新材料技术有限公司 | Preparation method of hard elastic polypropylene film, hard elastic polypropylene film and application |
| CN113741375A (en) * | 2021-09-18 | 2021-12-03 | 中国科学院近代物理研究所 | Special production terminal control system for heavy ion microporous membrane |
| CN113741375B (en) * | 2021-09-18 | 2023-02-03 | 中国科学院近代物理研究所 | Special production terminal control system for heavy ion microporous membrane |
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Denomination of invention: Preparation method of polyolefin microporous membrane Effective date of registration: 20230911 Granted publication date: 20120530 Pledgee: Cangzhou Branch of China Everbright Bank Co.,Ltd. Pledgor: CANGZHOU MINGZHU SEPARATOR TECHNOLOGY Co.,Ltd. Registration number: Y2023980056224 |