CN106751431A - A kind of battery separator and preparation method thereof - Google Patents
A kind of battery separator and preparation method thereof Download PDFInfo
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- CN106751431A CN106751431A CN201611196290.7A CN201611196290A CN106751431A CN 106751431 A CN106751431 A CN 106751431A CN 201611196290 A CN201611196290 A CN 201611196290A CN 106751431 A CN106751431 A CN 106751431A
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- carbon dioxide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 26
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 16
- 239000003063 flame retardant Substances 0.000 claims abstract description 16
- 239000005011 phenolic resin Substances 0.000 claims abstract description 16
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 16
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 15
- 230000000979 retarding effect Effects 0.000 claims abstract description 15
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims abstract description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 239000003365 glass fiber Substances 0.000 claims abstract description 11
- 239000011258 core-shell material Substances 0.000 claims abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 77
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 38
- 239000001569 carbon dioxide Substances 0.000 claims description 38
- 239000002904 solvent Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical group C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 3
- 229910052794 bromium Inorganic materials 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 3
- 125000005543 phthalimide group Chemical class 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical group 0.000 claims description 3
- 239000003017 thermal stabilizer Substances 0.000 claims description 3
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims description 3
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 3
- 229960004424 carbon dioxide Drugs 0.000 claims 7
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 2
- 229910002090 carbon oxide Inorganic materials 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OBXUKZGSGNXPSH-UHFFFAOYSA-N 2-phenoxy-1,3,5-triazine Chemical class N=1C=NC=NC=1OC1=CC=CC=C1 OBXUKZGSGNXPSH-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/18—Plasticising macromolecular compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C08J2433/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/53—Core-shell polymer
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of battery separator and preparation method thereof, the battery separator is mainly prepared from by the component of following weight part ratio：64.2 65 parts of 200 glass fibre plains of EW；29.8 30.2 parts of phenolic resin；0.1 0.7 parts of coupling agent；5 15 parts of heat stabilizer；0.5 5 parts of chemicals-resistant modifying agent；4.6 5.8 parts of barium titanate powder；26 parts of fire retarding synergist；5 15 parts of bromide fire retardant；36 parts of core-shell acrylic elastic emulsion.Gained dividing plate of the invention has light weight, intensity high, high temperature resistant, corrosion resistant advantage, and with preferable resistance to anti-flammability and toughness.
Description
Technical field
The present invention relates to a kind of battery separator and preparation method thereof, belong to field of chemical power source.
Background technology
Lead-acid accumulator is widely used, and worldwide output value yield all occupies all kinds of electrochmical power sources first places, generation therein
Table battery is analysing valve control type lead-acid accumulator battery.This lead-acid accumulator relies on two kinds of different mode fixed electrolytes, and one kind is AGM
Technology, i.e., by AGM dividing plate fixed electrolytes, most domestic lead-acid accumulator all uses this kind of technology now, but it has dividing plate
Aperture is too big, pressure-resistant performance is bad, the shortcomings of be easily caused acid layering, gradually by the more advanced colloid technique for fixing of another kind
Instead of.
Current dividing plate generally existing toughness is looked into, heat resistance is poor, the defect of decay resistance and resistance to poor flame retardant properties.
The content of the invention
The purpose of the present invention is directed to deficiency of the prior art, there is provided a kind of battery separator and preparation method thereof, institute
Obtaining dividing plate has light weight, intensity high, high temperature resistant, corrosion resistant advantage, and with preferable resistance to anti-flammability and toughness.
To achieve the above object, the present invention is adopted the technical scheme that：
A kind of battery separator, is mainly prepared from by the component of following weight part ratio：
64.2-65 parts of EW-200 glass fibre plains；Phenolic resin 29.8-30.2 parts；Coupling agent 0.1-0.7 parts；It is hot steady
Determine agent 5-15 parts；0.5-5 parts of chemicals-resistant modifying agent；Barium titanate powder 4.6-5.8 parts；Fire retarding synergist 2-6 parts；Bromine system is fire-retardant
Agent 5-15 parts；3-6 parts of core-shell acrylic elastic emulsion.
Preferably, described bromide fire retardant be tetrabromobisphenol A, TDE, 2,4,6- tribromo triple phenoxyl -1,
3,5- triazines, ethylidene-(double tetrabromo phthalimides), brominated epoxy, tetrabromophthalate-(2- ethylhexyls)
One or more in ester.
Preferably, described fire retarding synergist is Firebrake ZB, antimony oxide, antimony pentoxide, sodium antimonate and molybdenum oxide
In one or more material mixture.
Preferably, described chemicals-resistant modifying agent is the acrylic acid series additive containing perfluoroalkyl.
Preferably, the heat stabilizer is one or two the group in rare earth thermal stabilizer and organic tin heat stabilizer
Close.
The invention provides a kind of preparation method of battery separator, comprise the following steps:
S1, each component is weighed respectively according to a kind of formula of battery separator described in claim 1-5；
S2, barium titanate and 95% alcohol solvent are mixed, and use ultrasonically treated 2h；
S3, toward adding coupling agent in the mixed liquor of gained in step S2, and be heated to 70 DEG C of insulation 2h, heat while stirring；
S4, by the mixed liquor drying obtained by step S3, obtain the modified barium titanate powder in surface；
S5, the heat stabilizer that will be weighed, chemicals-resistant modifying agent, fire retarding synergist, bromide fire retardant, core-shell acrylic elasticity
Emulsion and step S4 obtain barium titanate powder and throw into double screw extruder, control screw speed for 180-600rpm, will
Liquid carbon dioxide is filled with delivery pump, wherein it is possible to be controlled the discharge pressure of carbon dioxide by the pressure that pressure valve sets
In critical pressure（7.4MPa）Any constant pressure in the range of to 50MPa heats the carbon dioxide so as to transport of carbon dioxide
To critical-temperature（31℃）Or higher temperature is to be translated into supercritical carbon dioxide, then by supercritical carbon dioxide
It is injected separately into the area of extruder three-four and five-eight areas, by melting extrusion, is crushed, obtains mix powder；
Mix powder obtained by S6, step S5 is added and is dissolved in the phenolic resin in alcohol solvent, is well mixed,
S7, by the metatitanic acid ba phenolic resin solvent obtained by EW-200 glass fibres plain immersion step S6, obtain prepreg；
S8, by the prepreg obtained by step S7 through laying, solidification obtains product.
Preferably, described double screw extruder includes 10 temperature controlled regions, and the temperature in temperature control 1-2 areas is 180-260 DEG C, temperature
The temperature in control 3-4 areas is 180-260 DEG C, and the temperature in temperature control 5-6 areas is 180-260 DEG C, and the temperature in temperature control 7-8 areas is 180-260
DEG C, the temperature in temperature control 9-10 areas is 180-260 DEG C, and the pressure in each area is 2-35MPa.
Preferably, stream of supercritical carbon dioxide speed is 1mL/min-50mL/min in described S3.
Preferably, the double screw extruder is provided with two and vacuumizes place, and end, the melting of material conveying section are located at one
The starting end of section, another place is located at metering section.
The invention has the advantages that：
Gained dividing plate has light weight, intensity high, high temperature resistant, corrosion resistant advantage, employs overage boundary's carbon dioxide injection treatment
Method, on the one hand, due to carbon dioxide non-toxic and safe, critical-temperature is low while have cost advantage, and it can it is swelling or
Person dissolves most polymers, and supercritical carbon dioxide has very strong plasticization to polymer, it is possible to reduce in material processing
When because the material degradation that causes of shearing force, reduce the generation of small molecular organic compounds；On the other hand, at vacuum port
Due to pressure reduction, supercritical carbon dioxide can gasify from vacuum port discharge, while taking the small molecule of dissolving out of, play reduction body
The effect of low-molecular material in system；By the addition of fire retardant and fire retarding synergist so that dividing plate has good anti-flammability, resistance toization
The addition of product modifying agent so that dividing plate has good anticorrosive property.
Specific embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with and it is specific real
Example is applied to be described in detail.
In following examples, the bromide fire retardant for being used is tetrabromobisphenol A, TDE, 2,4,6- tribromos three
Phenoxy group -1,3,5-triazines, ethylidene-(double tetrabromo phthalimides), brominated epoxy, tetrabromophthalate-(2-
Ethylhexyl) one or more in ester.
The fire retarding synergist for being used is in Firebrake ZB, antimony oxide, antimony pentoxide, sodium antimonate and molybdenum oxide
The mixture of kind or many kinds of substance.
The chemicals-resistant modifying agent for being used is the acrylic acid series additive containing perfluoroalkyl.
The heat stabilizer for being used is one or two the combination in rare earth thermal stabilizer and organic tin heat stabilizer.
Embodiment 1
S1, weigh 64.2 parts of EW-200 glass fibres plain；29.8 parts of phenolic resin；0.1 part of coupling agent；Heat stabilizer 5
Part；0.5 part of chemicals-resistant modifying agent；4.6 parts of barium titanate powder；2 parts of fire retarding synergist；5 parts of bromide fire retardant；Nucleocapsid propylene
3 parts of sour elastic emulsion；
S2, barium titanate and 95% alcohol solvent are mixed, and use ultrasonically treated 2h；
S3, toward adding coupling agent in the mixed liquor of gained in step S2, and be heated to 70 DEG C of insulation 2h, heat while stirring；
S4, by the mixed liquor drying obtained by step S3, obtain the modified barium titanate powder in surface；
S5, the heat stabilizer that will be weighed, chemicals-resistant modifying agent, fire retarding synergist, bromide fire retardant, core-shell acrylic elasticity
Emulsion and step S4 obtain barium titanate powder and throw into double screw extruder, control screw speed for 180-600rpm, will
Liquid carbon dioxide is filled with delivery pump, wherein it is possible to be controlled the discharge pressure of carbon dioxide by the pressure that pressure valve sets
In critical pressure（7.4MPa）Any constant pressure in the range of to 50MPa heats the carbon dioxide so as to transport of carbon dioxide
To critical-temperature（31℃）Or higher temperature is to be translated into supercritical carbon dioxide, then by supercritical carbon dioxide
It is injected separately into the area of extruder three-four and five-eight areas, by melting extrusion, is crushed, obtains mix powder；
Mix powder obtained by S6, step S5 is added and is dissolved in the phenolic resin in alcohol solvent, is well mixed,
S7, by the metatitanic acid ba phenolic resin solvent obtained by EW-200 glass fibres plain immersion step S6, obtain prepreg；
S8, by the prepreg obtained by step S7 through laying, solidification obtains product.
Described double screw extruder includes 10 temperature controlled regions, and the temperature in temperature control 1-2 areas is 180-260 DEG C, temperature control 3-4 areas
Temperature be 180-260 DEG C, the temperature in temperature control 5-6 areas is 180-260 DEG C, and the temperature in temperature control 7-8 areas is 180-260 DEG C, temperature control
The temperature in 9-10 areas is 180-260 DEG C, and the pressure in each area is 2-35MPa.
Stream of supercritical carbon dioxide speed is 1mL/min-50mL/min in described S3.
The double screw extruder is provided with two and vacuumizes place, the end of material conveying section, melt zone is located at one and is opened
Top, another place is located at metering section.
Embodiment 2
S1, weigh 65 parts of EW-200 glass fibres plain；30.2 parts of phenolic resin；0.7 part of coupling agent；Heat stabilizer 15
Part；5 parts of chemicals-resistant modifying agent；5.8 parts of barium titanate powder；6 parts of fire retarding synergist；15 parts of bromide fire retardant；Core-shell acrylic
6 parts of elastic emulsion；
S2, barium titanate and 95% alcohol solvent are mixed, and use ultrasonically treated 2h；
S3, toward adding coupling agent in the mixed liquor of gained in step S2, and be heated to 70 DEG C of insulation 2h, heat while stirring；
S4, by the mixed liquor drying obtained by step S3, obtain the modified barium titanate powder in surface；
S5, the heat stabilizer that will be weighed, chemicals-resistant modifying agent, fire retarding synergist, bromide fire retardant, core-shell acrylic elasticity
Emulsion and step S4 obtain barium titanate powder and throw into double screw extruder, control screw speed for 180-600rpm, will
Liquid carbon dioxide is filled with delivery pump, wherein it is possible to be controlled the discharge pressure of carbon dioxide by the pressure that pressure valve sets
In critical pressure（7.4MPa）Any constant pressure in the range of to 50MPa heats the carbon dioxide so as to transport of carbon dioxide
To critical-temperature（31℃）Or higher temperature is to be translated into supercritical carbon dioxide, then by supercritical carbon dioxide
It is injected separately into the area of extruder three-four and five-eight areas, by melting extrusion, is crushed, obtains mix powder；
Mix powder obtained by S6, step S5 is added and is dissolved in the phenolic resin in alcohol solvent, is well mixed,
S7, by the metatitanic acid ba phenolic resin solvent obtained by EW-200 glass fibres plain immersion step S6, obtain prepreg；
S8, by the prepreg obtained by step S7 through laying, solidification obtains product.
Described double screw extruder includes 10 temperature controlled regions, and the temperature in temperature control 1-2 areas is 180-260 DEG C, temperature control 3-4 areas
Temperature be 180-260 DEG C, the temperature in temperature control 5-6 areas is 180-260 DEG C, and the temperature in temperature control 7-8 areas is 180-260 DEG C, temperature control
The temperature in 9-10 areas is 180-260 DEG C, and the pressure in each area is 2-35MPa.
Stream of supercritical carbon dioxide speed is 1mL/min-50mL/min in described S3.
The double screw extruder is provided with two and vacuumizes place, the end of material conveying section, melt zone is located at one and is opened
Top, another place is located at metering section.
Embodiment 3
S1, weigh 64.6 parts of EW-200 glass fibres plain；30 parts of phenolic resin；0.4 part of coupling agent；Heat stabilizer 10
Part；2.75 parts of chemicals-resistant modifying agent；5.2 parts of barium titanate powder；4 parts of fire retarding synergist；10 parts of bromide fire retardant；Nucleocapsid propylene
4.5 parts of sour elastic emulsion；
S2, barium titanate and 95% alcohol solvent are mixed, and use ultrasonically treated 2h；
S3, toward adding coupling agent in the mixed liquor of gained in step S2, and be heated to 70 DEG C of insulation 2h, heat while stirring；
S4, by the mixed liquor drying obtained by step S3, obtain the modified barium titanate powder in surface；
S5, the heat stabilizer that will be weighed, chemicals-resistant modifying agent, fire retarding synergist, bromide fire retardant, core-shell acrylic elasticity
Emulsion and step S4 obtain barium titanate powder and throw into double screw extruder, control screw speed for 180-600rpm, will
Liquid carbon dioxide is filled with delivery pump, wherein it is possible to be controlled the discharge pressure of carbon dioxide by the pressure that pressure valve sets
In critical pressure（7.4MPa）Any constant pressure in the range of to 50MPa heats the carbon dioxide so as to transport of carbon dioxide
To critical-temperature（31℃）Or higher temperature is to be translated into supercritical carbon dioxide, then by supercritical carbon dioxide
It is injected separately into the area of extruder three-four and five-eight areas, by melting extrusion, is crushed, obtains mix powder；
Mix powder obtained by S6, step S5 is added and is dissolved in the phenolic resin in alcohol solvent, is well mixed；
S7, by the metatitanic acid ba phenolic resin solvent obtained by EW-200 glass fibres plain immersion step S6, obtain prepreg；
S8, by the prepreg obtained by step S7 through laying, solidification obtains product.
Described double screw extruder includes 10 temperature controlled regions, and the temperature in temperature control 1-2 areas is 180-260 DEG C, temperature control 3-4 areas
Temperature be 180-260 DEG C, the temperature in temperature control 5-6 areas is 180-260 DEG C, and the temperature in temperature control 7-8 areas is 180-260 DEG C, temperature control
The temperature in 9-10 areas is 180-260 DEG C, and the pressure in each area is 2-35MPa.
Stream of supercritical carbon dioxide speed is 1mL/min-50mL/min in described S3.
The double screw extruder is provided with two and vacuumizes place, the end of material conveying section, melt zone is located at one and is opened
Top, another place is located at metering section.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of battery separator, it is characterised in that be mainly prepared from by the component of following weight part ratio：
64.2-65 parts of EW-200 glass fibre plains；Phenolic resin 29.8-30.2 parts；Coupling agent 0.1-0.7 parts；It is hot steady
Determine agent 5-15 parts；0.5-5 parts of chemicals-resistant modifying agent；Barium titanate powder 4.6-5.8 parts；Fire retarding synergist 2-6 parts；Bromine system is fire-retardant
Agent 5-15 parts；3-6 parts of core-shell acrylic elastic emulsion.
2. a kind of battery separator according to claim 1, it is characterised in that described bromide fire retardant is tetrabromobisphenol
A, TDE, 2,4,6- tribromo triple phenoxyls -1,3,5-triazines, ethylidene-(double tetrabromo phthalimides), bromine
Change one or more in epoxy, tetrabromophthalate-(2- ethylhexyls) ester.
3. a kind of battery separator according to claim 1, it is characterised in that described fire retarding synergist be Firebrake ZB,
The mixture of one or more material in antimony oxide, antimony pentoxide, sodium antimonate and molybdenum oxide.
4. a kind of battery separator according to claim 1, it is characterised in that described chemicals-resistant modifying agent be containing
The acrylic acid series additive of perfluoroalkyl.
5. a kind of battery separator according to claim 1, it is characterised in that the heat stabilizer is rare earth thermal stabilizer
With one or two the combination in organic tin heat stabilizer.
6. a kind of preparation method of battery separator, it is characterised in that comprise the following steps:
S1, each component is weighed respectively according to a kind of formula of battery separator described in claim 1-5；
S2, barium titanate and 95% alcohol solvent are mixed, and use ultrasonically treated 2h；
S3, toward adding coupling agent in the mixed liquor of gained in step S2, and be heated to 70 DEG C of insulation 2h, heat while stirring；
S4, by the mixed liquor drying obtained by step S3, obtain the modified barium titanate powder in surface；
S5, the heat stabilizer that will be weighed, chemicals-resistant modifying agent, fire retarding synergist, bromide fire retardant, core-shell acrylic elasticity
Emulsion and step S4 obtain barium titanate powder and throw into double screw extruder, control screw speed for 180-600rpm, will
Liquid carbon dioxide is filled with delivery pump, wherein it is possible to be controlled the discharge pressure of carbon dioxide by the pressure that pressure valve sets
In critical pressure（7.4MPa）Any constant pressure in the range of to 50MPa heats the carbon dioxide so as to transport of carbon dioxide
To critical-temperature（31℃）Or higher temperature is to be translated into supercritical carbon dioxide, then by supercritical carbon dioxide
It is injected separately into the area of extruder three-four and five-eight areas, by melting extrusion, is crushed, obtains mix powder；
Mix powder obtained by S6, step S5 is added and is dissolved in the phenolic resin in alcohol solvent, is well mixed,
S7, by the metatitanic acid ba phenolic resin solvent obtained by EW-200 glass fibres plain immersion step S6, obtain prepreg；
S8, by the prepreg obtained by step S7 through laying, solidification obtains product.
7. a kind of preparation method of battery separator as claimed in claim 6, it is characterised in that described double screw extruder
Including 10 temperature controlled regions, the temperature in temperature control 1-2 areas is 180-260 DEG C, and the temperature in temperature control 3-4 areas is 180-260 DEG C, temperature control 5-6
The temperature in area is 180-260 DEG C, and the temperature in temperature control 7-8 areas is 180-260 DEG C, and the temperature in temperature control 9-10 areas is 180-260 DEG C, respectively
The pressure in area is 2-35MPa.
8. a kind of preparation method of battery separator as claimed in claim 6, it is characterised in that overcritical two in described S3
Carbonoxide flow velocity is 1mL/min-50mL/min.
9. a kind of preparation method of battery separator as claimed in claim 6, it is characterised in that on the double screw extruder
It is provided with two and vacuumizes place, end, the starting end of melt zone of material conveying section are located at one, another place is located at metering section.
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| CN201611196290.7A CN106751431A (en) | 2016-12-22 | 2016-12-22 | A kind of battery separator and preparation method thereof |
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Application publication date: 20170531 |