CN104617246B - A kind of preparation method of battery diaphragm - Google Patents
A kind of preparation method of battery diaphragm Download PDFInfo
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- CN104617246B CN104617246B CN201510086147.1A CN201510086147A CN104617246B CN 104617246 B CN104617246 B CN 104617246B CN 201510086147 A CN201510086147 A CN 201510086147A CN 104617246 B CN104617246 B CN 104617246B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005096 rolling process Methods 0.000 claims abstract description 23
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 20
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 20
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 20
- -1 polyoxyethylene Polymers 0.000 claims abstract description 20
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 10
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 10
- 239000000194 fatty acid Substances 0.000 claims abstract description 10
- 229930195729 fatty acid Natural products 0.000 claims abstract description 10
- 239000003365 glass fiber Substances 0.000 claims abstract description 10
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960003943 hypromellose Drugs 0.000 claims abstract description 10
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims abstract description 10
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 10
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052756 noble gas Inorganic materials 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 238000003490 calendering Methods 0.000 description 7
- 210000004027 cell Anatomy 0.000 description 7
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention discloses the preparation method of a kind of battery diaphragm; first by epoxy resin; glass fibre; tungsten dioxide; citric acid and polyvinyl alcohol are uniformly mixed, and are subsequently adding in reactor, and under the conditions of inert gas shielding, heated and stirred adds polyoxyethylene isobutyl group 2, 2-Oxydiphenol and hypromellose; heating keeps 30 40 minutes under vacuum, obtains intermedium one；Again intermedium one is rolled film forming by rolling process, then film is joined in deionized water, add dehydrated alcohol, ammonium hydrogen phosphate, polyglyceryl fatty acid ester, dodecylbenzene sodium sulfonate, hydroxypropyl methyl cellulose, it is heated to boiling, and keep 15 20 minutes, it is down to room temperature, obtains battery diaphragm.The battery diaphragm that the present invention provides has good combination property, the significant increase using value of barrier film.
Description
Technical field
The invention belongs to battery material preparing technical field, be specifically related to the preparation method of a kind of battery diaphragm.
Background technology
In recent years, along with highlighting of the problems such as the day by day exhausted of resource and global warming, the life style of green low-carbon receives to be advocated.Wherein, development electric motor car and hybrid electric vehicle partly replace the internal-combustion engines vehicle of consumption of fossil fuels to be one of main method solving energy crisis and ecological deterioration.Driving power supply is to affect the critical component that electric motor car is promoted the use of, and the most widely used driving power supply includes lead-acid battery, nickel-cadmium cell (NiCd), lithium ion battery and zinc-nickel cell etc..In various driving power supplys, zinc-nickel cell, owing to having the advantages such as power height, energy foot, non-environmental-pollution, reliability height and safety is good, with low cost, length in service life, has obtained studying widely.In zinc-nickel cell, deformation, dendrite easily occur due to zincode, corrodes and the problem such as passivation, thus cycle life is short, self discharge is relatively big and recycles the defects such as process capacities decay is fast to cause zinc-nickel cell to exist.In order to improve the drawbacks described above of zinc-nickel cell, zinc-nickel cell barrier film is constantly studied by related researcher.Having had research to improve disadvantages described above at present, but conventional battery diaphragm there is also mechanical strength not, wellability is poor, the problem of septal perforator, is therefore accomplished by further researching and developing the battery diaphragm of a kind of high comprehensive performance.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of battery diaphragm to solve above the deficiencies in the prior art, prepared the battery diaphragm of excellent combination property by ad hoc approach.
The technological means that the present invention uses is as follows:
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, joins in mixing and blending machine by epoxy resin 20-30 part, glass fibre 3-8 part, tungsten dioxide 1-4 part, citric acid 2-8 part and polyvinyl alcohol 5-10 part, is uniformly mixed, obtains mixed material；
Step 2; mixed material is added in reactor; 130-150 DEG C it is heated under the conditions of inert gas shielding; stir 40-60 minute; it is subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 2-5 part and hypromellose 3-8 part; it is heated to 100-120 DEG C under vacuum, keeps 30-40 minute, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, then film is joined in the deionized water that mass parts is 300-400 part, add dehydrated alcohol 10-20 part, ammonium hydrogen phosphate 3-8 part, polyglyceryl fatty acid ester 1-5 part, dodecylbenzene sodium sulfonate 2-5 part, hydroxypropyl methyl cellulose 1-4 part, it is heated to boiling, and keep 15-20 minute, it is down to room temperature, obtains battery diaphragm.
Further, the preparation method of described battery diaphragm, stirring mixing condition in step 1 is whipping temp 60-70 DEG C, mixing speed 150-180 rev/min, mixing time 30-40 minute.
Further, the preparation method of described battery diaphragm, noble gas described in step 2 is nitrogen or argon.
Further, the preparation method of described battery diaphragm, the vacuum of vacuum condition described in step 2 is 0.02-0.06MPa.
Further, the preparation method of described battery diaphragm, in step 3, rolling condition is melting temperature 180-190 DEG C, rolling temperature 180-200 DEG C.
Further, the preparation method of described battery diaphragm, the process being down to room temperature in step 3 is first to be down to 0 DEG C with the speed of 30-35 DEG C/min, keeps 10-20 minute, warms naturally to room temperature the most again.
Further, the preparation method of described battery diaphragm, the thickness rolling caudacoria in step 3 is 800-1000 μm.
The battery diaphragm that the present invention provides has good combination property, and wherein pick up has reached more than 192%, and gain in weight has reached 4.8
g/m2Above, surface resistance has reached 0.017 Ω/cm2Hereinafter, hot strength has reached more than 162MPa, and overall performance is excellent.The present invention has obtained the separator product of superior performance by specific step, the significant increase using value of barrier film.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 20 parts, glass fibre 3 parts, tungsten dioxide 1 part, citric acid 2 parts and polyvinyl alcohol 5 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 60 DEG C, mixing speed 150 revs/min, mixing time 30 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 130 DEG C under nitrogen protective condition; stir 40 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 2 parts and hypromellose 3 parts, at the heated under vacuum that vacuum is 0.02MPa to 100 DEG C; keep 30 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 180 DEG C, rolling temperature 180 DEG C, the thickness of calendering caudacoria is 800 μm, then film is joined in the deionized water that mass parts is 300 parts, add dehydrated alcohol 10 parts, ammonium hydrogen phosphate 3 parts, polyglyceryl fatty acid ester 1 part, dodecylbenzene sodium sulfonate 2 parts, hydroxypropyl methyl cellulose 1 part, it is heated to boiling, and keep 15 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 30 DEG C/min, keep 10 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
Embodiment 2
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 23 parts, glass fibre 5 parts, tungsten dioxide 2 parts, citric acid 4 parts and polyvinyl alcohol 6 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 63 DEG C, mixing speed 160 revs/min, mixing time 35 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 136 DEG C under the conditions of argon shield; stir 50 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 3 parts and hypromellose 5 parts, at the heated under vacuum that vacuum is 0.03MPa to 110 DEG C; keep 35 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 183 DEG C, rolling temperature 188 DEG C, the thickness of calendering caudacoria is 800 μm, then film is joined in the deionized water that mass parts is 330 parts, add dehydrated alcohol 13 parts, ammonium hydrogen phosphate 5 parts, polyglyceryl fatty acid ester 2 parts, dodecylbenzene sodium sulfonate 3 parts, hydroxypropyl methyl cellulose 2 parts, it is heated to boiling, and keep 18 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 32 DEG C/min, keep 15 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
Embodiment 3
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 26 parts, glass fibre 7 parts, tungsten dioxide 3 parts, citric acid 6 parts and polyvinyl alcohol 8 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 68 DEG C, mixing speed 170 revs/min, mixing time 37 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 145 DEG C under nitrogen protective condition; stir 50 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 4 parts and hypromellose 6 parts, at the heated under vacuum that vacuum is 0.04MPa to 115 DEG C; keep 36 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 185 DEG C, rolling temperature 194 DEG C, the thickness of calendering caudacoria is 870 μm, then film is joined in the deionized water that mass parts is 360 parts, add dehydrated alcohol 18 parts, ammonium hydrogen phosphate 7 parts, polyglyceryl fatty acid ester 4 parts, dodecylbenzene sodium sulfonate 3 parts, hydroxypropyl methyl cellulose 3 parts, it is heated to boiling, and keep 18 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 34 DEG C/min, keep 18 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
Embodiment 4
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 30 parts, glass fibre 8 parts, tungsten dioxide 4 parts, citric acid 8 parts and polyvinyl alcohol 10 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 70 DEG C, mixing speed 180 revs/min, mixing time 40 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 150 DEG C under nitrogen protective condition; stir 60 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 5 parts and hypromellose 8 parts, at the heated under vacuum that vacuum is 0.06MPa to 120 DEG C; keep 40 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 190 DEG C, rolling temperature 200 DEG C, the thickness of calendering caudacoria is 1000 μm, then film is joined in the deionized water that mass parts is 400 parts, add dehydrated alcohol 20 parts, ammonium hydrogen phosphate 8 parts, polyglyceryl fatty acid ester 5 parts, dodecylbenzene sodium sulfonate 5 parts, hydroxypropyl methyl cellulose 4 parts, it is heated to boiling, and keep 20 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 35 DEG C/min, keep 20 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
Comparative example 1
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 26 parts, glass fibre 7 parts, citric acid 6 parts and polyvinyl alcohol 8 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 68 DEG C, mixing speed 170 revs/min, mixing time 37 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 145 DEG C under nitrogen protective condition; stir 50 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 4 parts and hypromellose 6 parts, at the heated under vacuum that vacuum is 0.04MPa to 115 DEG C; keep 36 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 185 DEG C, rolling temperature 194 DEG C, the thickness of calendering caudacoria is 870 μm, then film is joined in the deionized water that mass parts is 360 parts, add dehydrated alcohol 18 parts, ammonium hydrogen phosphate 7 parts, polyglyceryl fatty acid ester 4 parts, dodecylbenzene sodium sulfonate 3 parts, hydroxypropyl methyl cellulose 3 parts, it is heated to boiling, and keep 18 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 34 DEG C/min, keep 18 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
Comparative example 2
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 26 parts, glass fibre 7 parts, tungsten dioxide 3 parts, citric acid 6 parts and polyvinyl alcohol 8 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 68 DEG C, mixing speed 170 revs/min, mixing time 37 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 145 DEG C under nitrogen protective condition; stir 50 minutes, be subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 4 parts and hypromellose 6 parts, at the heated under vacuum that vacuum is 0.04MPa to 115 DEG C; keep 36 minutes, obtain intermedium one；
Step 3, rolls film forming by intermedium one by rolling process, and wherein melting temperature is 185 DEG C, rolling temperature 194 DEG C, the thickness of calendering caudacoria is 870 μm, is then joined by film in the deionized water that mass parts is 360 parts, add dehydrated alcohol 18 parts, ammonium hydrogen phosphate 7 parts, polyglyceryl fatty acid ester 4 parts, dodecylbenzene sodium sulfonate 3 parts, hydroxypropyl methyl cellulose 3 parts, is heated to boiling, and keeps 18 minutes, naturally it is down to room temperature, obtains battery diaphragm.
Comparative example 3
The preparation method of a kind of battery diaphragm, comprises the following steps:
Step 1, according to weight portion, by epoxy resin 26 parts, glass fibre 7 parts, tungsten dioxide 3 parts, citric acid 6 parts and polyvinyl alcohol 8 parts join in mixing and blending machine, are uniformly mixed, and condition is whipping temp 68 DEG C, mixing speed 170 revs/min, mixing time 37 minutes, obtain mixed material；
Step 2, adds mixed material in reactor, is heated to 145 DEG C under nitrogen protective condition, stirs 50 minutes, is subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 4 parts and hypromellose 6 parts, is heated to 115 DEG C, keeps 36 minutes, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, wherein melting temperature is 185 DEG C, rolling temperature 194 DEG C, the thickness of calendering caudacoria is 870 μm, then film is joined in the deionized water that mass parts is 360 parts, add dehydrated alcohol 18 parts, ammonium hydrogen phosphate 7 parts, polyglyceryl fatty acid ester 4 parts, dodecylbenzene sodium sulfonate 3 parts, hydroxypropyl methyl cellulose 3 parts, it is heated to boiling, and keep 18 minutes, it is down to room temperature, the process being down to room temperature is first to be down to 0 DEG C with the speed of 34 DEG C/min, keep 18 minutes, warm naturally to room temperature the most again, obtain battery diaphragm.
The battery diaphragm preparing above example and comparative example carries out performance test, result such as following table:
From above test data it can be seen that the battery diaphragm that the present invention provides has good combination property, wherein pick up has reached more than 192%, and gain in weight has reached 4.8 g/m2Above, surface resistance has reached 0.017 Ω/cm2Hereinafter, hot strength has reached more than 162MPa, and overall performance is excellent.Wherein the result of embodiment 3 is the most prominent, therefore can be as most preferred embodiment.Comparative example 1-3 is all the proving test carried out on the basis of embodiment 3, does not wherein add tungsten dioxide in comparative example 1, and result causes surface resistance greatly to raise, and illustrates that the introducing of this component can reduce surface resistance；The process being down to room temperature in comparative example 2 in step 2 is: be first down to 0 DEG C with the speed of 34 DEG C/min, keep 18 minutes removing, result causes battery diaphragm hot strength substantially to reduce, surface resistance also has certain rising, and the step therefore lowered the temperature has material impact for mechanical strength and the surface resistance of final barrier film；Not using vacuum condition in comparative example 3 in preparation process 2, result causes pick up and the gain in weight considerable decrease of barrier film, and therefore this condition is the important step of the barrier film that can obtain the good present invention of pick up.
Claims (7)
1. the preparation method of a battery diaphragm, it is characterised in that comprise the following steps:
Step 1, according to weight portion, joins in mixing and blending machine by epoxy resin 20-30 part, glass fibre 3-8 part, tungsten dioxide 1-4 part, citric acid 2-8 part and polyvinyl alcohol 5-10 part, is uniformly mixed, obtains mixed material；
Step 2; mixed material is added in reactor; 130-150 DEG C it is heated under the conditions of inert gas shielding; stir 40-60 minute; it is subsequently adding polyoxyethylene isobutyl group 2, 2-Oxydiphenol 2-5 part and hypromellose 3-8 part; it is heated to 100-120 DEG C under vacuum, keeps 30-40 minute, obtain intermedium one；
Step 3, intermedium one is rolled film forming by rolling process, then film is joined in the deionized water that mass parts is 300-400 part, add dehydrated alcohol 10-20 part, ammonium hydrogen phosphate 3-8 part, polyglyceryl fatty acid ester 1-5 part, dodecylbenzene sodium sulfonate 2-5 part, hydroxypropyl methyl cellulose 1-4 part, it is heated to boiling, and keep 15-20 minute, it is down to room temperature, obtains battery diaphragm.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that stirring mixing condition in step 1 is whipping temp 60-70 DEG C, mixing speed 150-180 rev/min, mixing time 30-40 minute.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that noble gas described in step 2 is nitrogen or argon.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that the vacuum of vacuum condition described in step 2 is 0.02-0.06MPa.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that in step 3, rolling condition is melting temperature 180-190 DEG C, rolling temperature 180-200 DEG C.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that the process being down to room temperature in step 3 is first to be down to 0 DEG C with the speed of 30-35 DEG C/min, keeps 10-20 minute, warms naturally to room temperature the most again.
The preparation method of battery diaphragm the most according to claim 1, it is characterised in that the thickness rolling caudacoria in step 3 is 800-1000 μm.
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