JP2734617B2 - Manufacturing method of separator - Google Patents
Manufacturing method of separatorInfo
- Publication number
- JP2734617B2 JP2734617B2 JP1077802A JP7780289A JP2734617B2 JP 2734617 B2 JP2734617 B2 JP 2734617B2 JP 1077802 A JP1077802 A JP 1077802A JP 7780289 A JP7780289 A JP 7780289A JP 2734617 B2 JP2734617 B2 JP 2734617B2
- Authority
- JP
- Japan
- Prior art keywords
- separator
- water
- graft
- silver
- battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/42—Acrylic resins
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
-
- 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
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はセパレータの製造方法に関し、さらに詳しく
は、酸化銀電池などの電池内で銀イオンなどの陽極活物
質の透過阻止に優れた能力を発揮するセパレータの製造
方法に関する。Description: TECHNICAL FIELD The present invention relates to a method for producing a separator, and more particularly, to a method for preventing permeation of an anode active material such as silver ions in a battery such as a silver oxide battery. The present invention relates to a method for producing a separator that exerts its effect.
一般に電池用セパレータとしては、電気抵抗が小さ
く、かつ均一であることが求められている。このような
性質を有する電池用セパレータの製造方法として、例え
ば特開昭55−105963号公報には、ポリオレフィン膜にア
クリル酸等の親水性モノマーをグラフト重合したのち、
水酸化カリウム水溶液で処理する方法が知られている
が、銀イオンなどの陽極活物質の透過を阻止する機能を
付与すれば電池の寿命はさらに延びる。In general, a battery separator is required to have low and uniform electric resistance. As a method for producing a battery separator having such properties, for example, JP-A-55-105963 discloses that after graft-polymerizing a hydrophilic monomer such as acrylic acid on a polyolefin film,
A method of treating with a potassium hydroxide aqueous solution is known. However, if a function of preventing permeation of an anode active material such as silver ions is provided, the life of the battery is further extended.
本発明の目的は、酸化銀電池などの電池内で、銀イオ
ンなどの陽極活物質の透過阻止に優れた能力を発揮する
セパレータの製造方法を提案することである。An object of the present invention is to propose a method for producing a separator that exhibits excellent ability to prevent permeation of anode active materials such as silver ions in a battery such as a silver oxide battery.
本発明の他の目的は、耐ブロッキング性が良好で、電
池作成時の作業性の良いセパレータの製造方法を提案す
ることである。Another object of the present invention is to propose a method for producing a separator having good blocking resistance and good workability in battery production.
本発明に係るセパレータの製造方法は、ポリエチレン
を基材とし、この基材に（メタ）アクリル酸をグラフト
重合し、得られたグラフト膜を水酸化アルカリ水溶液で
中和し、次いで水と水溶性有機溶媒との混合液で洗浄す
ることを特徴とするセパレータの製造方法である。In the method for producing a separator according to the present invention, a polyethylene is used as a base material, (meth) acrylic acid is graft-polymerized on the base material, the obtained graft film is neutralized with an aqueous alkali hydroxide solution, and then water and water-soluble A method for producing a separator, comprising washing with a mixed solution with an organic solvent.
本発明において基材として用いるポリエチレンは、高
密度、中密度、または低密度ポリエチレンのいずれでも
良い。これらポリエチレンは、０〜10モル％の割合で炭
素数３〜20のα−オレフィンまたはビニルモノマーをコ
モノマーとして含有していてもよい。α−オレフィンと
してはプロピレン、１−ブテン、１ヘキセン、４−メチ
ル−１−ペンテン、１−デセンなどをあげることができ
る。ビニルモノマーとしてはアクリル酸、メタクリル
酸、酢ルビニルなどをあげることができる。The polyethylene used as the base material in the present invention may be any of high density, medium density, or low density polyethylene. These polyethylenes may contain an α-olefin having 3 to 20 carbon atoms or a vinyl monomer as a comonomer at a ratio of 0 to 10 mol%. Examples of the α-olefin include propylene, 1-butene, 1-hexene, 4-methyl-1-pentene, 1-decene and the like. Examples of the vinyl monomer include acrylic acid, methacrylic acid, and vinyl acetate.
また、本発明に用いるポリエチレンは、デカリン溶媒
中135℃で測定した極限粘度〔η〕が通常0.5dl/g以上、
好ましくは1.0〜5.0dl/g、特に好ましくは2.0〜4.0dl/g
のものが適当である。Further, the polyethylene used in the present invention has an intrinsic viscosity (η) measured at 135 ° C. in a decalin solvent of usually 0.5 dl / g or more,
Preferably 1.0 to 5.0 dl / g, particularly preferably 2.0 to 4.0 dl / g
Is appropriate.
本発明において基材はフィルムの形で用いられる。こ
のような基材フィルムとして用いられるポリエチレン膜
は５〜100μｍ、好ましくは７〜40μｍ程度の膜厚を有
していることが電池容量および成形性の観点から好まし
い。In the present invention, the substrate is used in the form of a film. It is preferable that the polyethylene film used as such a base film has a thickness of about 5 to 100 μm, preferably about 7 to 40 μm from the viewpoint of battery capacity and moldability.
基材としてのポリエチレンに（メタ）アクリル酸をグ
ラフト重合するには、ポリエチレン膜に１〜30Mradの電
子線を照射した後、このポリエチレン膜を充分に脱気さ
れた５〜50重量％のアクリル酸および／またはメタクリ
ル酸水溶液中に、20〜50℃で１〜60分間浸漬してグラフ
ト重合を行う。To graft polymerize (meth) acrylic acid to polyethylene as a base material, the polyethylene film is irradiated with an electron beam of 1 to 30 Mrad, and then the polyethylene film is sufficiently degassed with 5 to 50% by weight of acrylic acid. And / or immersion in an aqueous methacrylic acid solution at 20 to 50 ° C. for 1 to 60 minutes to perform graft polymerization.
次に、このようにして得られたポリエチレンのグラフ
ト膜を水酸化アルカリ水溶液を浸漬して中和処理を行
う。この中和処理に使用する水酸化アルカリとしては水
酸化カリウム、水酸化ナトリウム等があげられるが、水
酸化カリウムが好ましい。中和処理に用いるアルカリ水
溶液の濃度は、セパレータとして装着されるアルカリ電
池の電解液としての水酸化アルカリ水溶液濃度をα重量
％とした場合、α±５重量％以内とするのが好ましい。
例えば装着される電池電解液としての水酸化カリウムの
濃度が40重量％である場合には、40±５重量％の水酸化
カリウム溶液を用いることが好ましい。グラフト膜のア
ルカリ水溶液による中和処理は、常温ないし70℃の温度
で、10〜60分間行うことが好ましい。Next, the polyethylene graft membrane thus obtained is immersed in an aqueous alkali hydroxide solution to perform a neutralization treatment. Examples of the alkali hydroxide used for the neutralization treatment include potassium hydroxide and sodium hydroxide, and potassium hydroxide is preferred. The concentration of the aqueous alkali solution used for the neutralization treatment is preferably within α ± 5% by weight when the concentration of the aqueous alkali hydroxide solution as the electrolytic solution of the alkaline battery mounted as the separator is α% by weight.
For example, when the concentration of potassium hydroxide as the battery electrolyte to be mounted is 40% by weight, it is preferable to use a 40 ± 5% by weight potassium hydroxide solution. The neutralization treatment of the graft membrane with an aqueous alkali solution is preferably performed at a temperature from room temperature to 70 ° C. for 10 to 60 minutes.
次に、このようにして水酸化アルカリ水溶液により中
和処理されたグラフト膜を、水と水溶性有機溶媒との混
合液で洗浄する。このような水溶性有機溶媒としては、
アルコール系、ケトン系およびカルボン酸系などの有機
溶媒をあげることができ、これらの有機溶媒の中でもメ
タノール、エタノール、エチレングリコールなどのアル
コール系有機溶媒、およびアセトンなどのケトン系有機
溶媒が好ましい。このような有機溶媒は、単独であるい
は２種以上混合して用いられるが、特にエチレングリコ
ールとメタノールと水との混合液が好ましい。Next, the graft membrane thus neutralized with the aqueous alkali hydroxide solution is washed with a mixture of water and a water-soluble organic solvent. As such a water-soluble organic solvent,
Organic solvents such as alcohols, ketones, and carboxylic acids can be used. Among these organic solvents, alcohol-based organic solvents such as methanol, ethanol, and ethylene glycol, and ketone-based organic solvents such as acetone are preferable. Such organic solvents are used alone or as a mixture of two or more, and a mixed solution of ethylene glycol, methanol and water is particularly preferred.
本発明で用いられる水溶性有機溶媒は、20℃における
水に対する溶解度が１体積％以上、好ましくは10体積％
以上、より好ましくは20体積％以上であることが望まし
く、特に完全相溶性の有機溶媒であることが望ましい。The water-soluble organic solvent used in the present invention has a solubility in water at 20 ° C. of 1% by volume or more, preferably 10% by volume.
As described above, the content is more preferably 20% by volume or more, and particularly preferably a completely compatible organic solvent.
本発明で用いられる水と水溶性有機溶媒との混合物に
おける水と水溶性有機溶媒との混合比は、重量比で5:95
〜95:5、好ましくは20:80〜80:20、特に好ましくは30:7
0〜70:30であることが望ましい。The mixing ratio of water and the water-soluble organic solvent in the mixture of water and the water-soluble organic solvent used in the present invention is 5:95 by weight.
~ 95: 5, preferably 20:80 to 80:20, particularly preferably 30: 7
Desirably, it is 0 to 70:30.
上記のような水と水溶性有機溶媒との混合液によりグ
ラフト膜を洗浄する際の洗浄温度は５〜70℃、好ましく
は常温以上50℃未満が望ましい。洗浄時間は１〜60分
間、好ましくは２〜５分間が望ましい。The washing temperature when the graft membrane is washed with a mixture of water and a water-soluble organic solvent as described above is preferably from 5 to 70 ° C, more preferably from room temperature to less than 50 ° C. The washing time is 1 to 60 minutes, preferably 2 to 5 minutes.
上記の水と水溶性有機溶媒との混合液によりグラフト
膜を洗浄するには、たとえばグラフト膜を上記の混合液
に浸漬する方法、上記混合液をシャワーする方法などが
ある。The method of washing the graft membrane with the above-mentioned mixed solution of water and a water-soluble organic solvent includes, for example, a method of dipping the graft film in the above-mentioned mixed solution, a method of showering the above-mentioned mixed solution, and the like.
上記の洗浄によりセパレータの製造は完了し、洗浄を
終ったグラフト膜はセパレータとして使用される。本発
明により製造されるセパレータは、銀イオン等の陽極活
物質の透過阻止を必要とする酸化銀電池など電池用のセ
パレータとして用いるのに適しているが、イオン等の透
過を阻止する他の用途のセパレータとしても用いること
ができる。By the above washing, the production of the separator is completed, and the graft membrane after the washing is used as a separator. The separator manufactured according to the present invention is suitable for use as a separator for batteries such as silver oxide batteries which require the prevention of permeation of anode active materials such as silver ions, but other uses for preventing permeation of ions etc. Can also be used as a separator.
本発明のセパレータは単独で、または複数枚を積層し
て、電池等のセパレータに用いることができるが、耐ブ
ロッキング性が優れているため、電池等の作成時の作業
性は良好である。The separator of the present invention can be used alone or in a laminate of a plurality of sheets to form a separator for a battery or the like. However, since the separator has excellent blocking resistance, the workability at the time of producing the battery and the like is good.
本発明に係るセパレータの製造方法では、ポリエチレ
ン膜を基材とし、このポリエチレン膜に（メタ）アクリ
ル酸をグラフト重合し、得られたグラフト膜を水酸化ア
ルカリ水酸化で中和し、次いで水と水溶性有機溶媒との
混合液で洗浄してセパレータを製造するため、銀イオン
などの陽極活物質の透過を阻止し、優れた特性を有する
セパレータが得られ、セパレータ自体の寿命が延びると
ともに、このセパレータが装着された電池等の寿命も延
びる。In the method for producing a separator according to the present invention, a polyethylene film is used as a base material, (meth) acrylic acid is graft-polymerized on the polyethylene film, the obtained graft film is neutralized with alkali hydroxide and then water. Since the separator is manufactured by washing with a mixed solution with a water-soluble organic solvent, permeation of anode active materials such as silver ions is prevented, and a separator having excellent characteristics is obtained. The life of a battery or the like to which the separator is attached is also extended.
また、得られたセパレータは耐ブロッキング性も良
く、電池等の作成の作業性も良くなる。In addition, the obtained separator has good blocking resistance, and the workability of producing a battery or the like is also improved.
以下、本発明を実施例により説明するが、本発明はこ
れら実施例に限定されるものではない。Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited to these examples.
実施例１ 高密度ポリエチレンフィルム（厚さ20μｍ、密度0.95
5、〔η〕3.2dl/g）に、電子線照射装置を用いて10Mrad
の電子線を窒素雰囲気下で冷却しながら照射した。次に
電子線の照射されたこのポリエチレン膜を、あらかじめ
充分に脱気され、かつモール塩が0.25重量％添加された
30重量％アクリル酸水溶液中に、40℃で10分間浸漬して
グラフト重合を行い、グラフト膜を得た。得られたグラ
フト膜のグラフト率は55％であった。Example 1 High-density polyethylene film (thickness 20 μm, density 0.95
5, [η] 3.2 dl / g) using an electron beam irradiation device at 10 Mrad
Was irradiated while cooling under a nitrogen atmosphere. Next, the polyethylene film irradiated with an electron beam was sufficiently degassed in advance, and 0.25% by weight of Mohr's salt was added.
Graft polymerization was performed by immersion in a 30% by weight aqueous solution of acrylic acid at 40 ° C. for 10 minutes to obtain a graft film. The graft ratio of the obtained graft membrane was 55%.
次にこのようにアクリル酸水溶液に浸漬して得られた
グラフト膜（Ｉ）を、40重量％水酸化カリウム水溶液に
40℃で10分間浸漬して中和処理し、次いでエチレングリ
コールとメタノールと水との混合比が1:5:4である水溶
液を用いて室温で洗浄し、次いで乾燥してセパレータ
（Ｉ）を得た。Next, the graft membrane (I) obtained by immersing in the acrylic acid aqueous solution in this manner is converted into a 40% by weight aqueous solution of potassium hydroxide.
A neutralization treatment was performed by immersion at 40 ° C. for 10 minutes, followed by washing at room temperature using an aqueous solution having a mixture ratio of ethylene glycol, methanol, and water of 1: 5: 4, followed by drying to obtain a separator (I). Obtained.
次にセパレータ（Ｉ）を酸化亜鉛飽和の30重量％水酸
化カリウム水溶液に浸漬してセパレータ（II）を得た。
次いでセパレータ（Ｉ）１枚とセパレータ（II）７枚と
を、セパレータ（Ｉ）が最上部にくるように積層してセ
パレータ積層体を得た。Next, the separator (I) was immersed in a 30% by weight aqueous solution of potassium hydroxide saturated with zinc oxide to obtain a separator (II).
Next, one separator (I) and seven separators (II) were laminated so that the separator (I) was at the uppermost position, to obtain a separator laminate.
このセパレータ積層体を第１図に示すような銀透過試
験用セルに装着して、各セパレータを透過した銀イオン
の量を測定した。なおセパレータ（II）は実際の電池の
状態に合わせるために、上記の含浸を行った。This separator laminate was attached to a cell for a silver permeation test as shown in FIG. 1, and the amount of silver ions transmitted through each separator was measured. The separator (II) was impregnated as described above in order to match the actual battery condition.
第１図に示す銀透過試験用セルにおいて、１はガラス
板、２はセパレータ積層体、３は壁面、４はシール部
材、５は酸化銀、６は30重量％水酸化カリウム水溶液、
７は空気抜きである。In the silver permeation test cell shown in FIG. 1, 1 is a glass plate, 2 is a separator laminate, 3 is a wall surface, 4 is a sealing member, 5 is silver oxide, 6 is a 30% by weight potassium hydroxide aqueous solution,
7 is an air vent.
このように形成した銀透過試験用セルを70℃で24時間
静置した後、セパレータ積層体２を取り出し、各セパレ
ータにおける銀の浸透状態を肉眼観察したところ、１枚
目のセパレータ（Ｉ）にだけ銀が浸透していたが２〜８
枚目のセパレータ（II）には銀は認められなかった。After the silver permeation test cell thus formed was allowed to stand at 70 ° C. for 24 hours, the separator laminate 2 was taken out, and the permeation state of silver in each separator was visually observed. Only silver penetrated, but 2-8
No silver was observed in the second separator (II).
また、各セパレータの銀の保持量をICP発光分析で測
定したところ、１枚目7205μｇ、２枚目35μｇ、３枚目
５μｇの銀が検知され、４枚目以後には、銀が検知され
なかった。When the amount of silver retained in each separator was measured by ICP emission analysis, 7205 μg of the first sheet, 35 μg of the second sheet, 5 μg of the third sheet were detected, and no silver was detected after the fourth sheet. Was.
比較例１ 実施例１で得られたグラフト膜（Ｉ）を純水で水洗し
た後、乾燥してセパレータ（III）を得た。このセパレ
ータ（III）に酸化亜鉛飽和の30重量％水酸化カリウム
水溶液を含浸させてセパレータ（IV）を得た。これらを
用いて実施例１と同様の試験を施したところ、銀は７枚
目まで観察された。Comparative Example 1 The graft membrane (I) obtained in Example 1 was washed with pure water and then dried to obtain a separator (III). This separator (III) was impregnated with a 30% by weight aqueous solution of potassium hydroxide saturated with zinc oxide to obtain a separator (IV). When a test similar to that of Example 1 was performed using these, silver was observed up to the seventh sheet.
また実施例１と同様に各セパレータの銀の保持量を測
定したところ、１枚目245μｇ、２枚目70μｇ、３枚目4
1μｇ、４枚目39μｇ、５枚目26μｇ、６枚目20μｇ、
７枚目21μｇ、８枚目21μｇの銀が検知された。When the amount of silver retained in each separator was measured in the same manner as in Example 1, the first sheet was 245 μg, the second sheet was 70 μg, and the third sheet was 4 μg.
1 μg, fourth 39 μg, fifth 26 μg, sixth 20 μg,
21 μg of the seventh sheet and 21 μg of the eighth sheet were detected.
第１図は実施例において銀透過試験に用いた銀透過試験
用セルの断面図である。 １……ガラス板、２……セパレータ積層体 ３……壁面FIG. 1 is a sectional view of a silver permeation test cell used in a silver permeation test in Examples. 1 ... glass plate, 2 ... separator laminate 3 ... wall surface
───────────────────────────────────────────────────── フロントページの続き (72)発明者 吉田 雅人 宮城県仙台市西多賀５―30―１ セイコ ー電子部品株式会社内 (56)参考文献 特開 昭64−65772（ＪＰ，Ａ) 特許2539860（ＪＰ，Ｃ１) 特許1231648（ＪＰ，Ｃ２) ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Masato Yoshida 5-30-1 Nishitaga, Sendai City, Miyagi Prefecture Seiko Electronic Components Co., Ltd. (56) References JP-A-64-65772 (JP, A) Patent 2539860 ( JP, C1) Patent 1231648 (JP, C2)
Claims (1)
タ）アクリル酸をグラフト重合し、得られたグラフト膜
を水酸化アルカリ水溶液で中和し、次いで水と水溶性有
機溶媒との混合液で洗浄することを特徴とするセパレー
タの製造方法。1. A method comprising the steps of: (1) using polyethylene as a base material, graft-polymerizing (meth) acrylic acid onto the base material, neutralizing the obtained graft film with an aqueous alkali hydroxide solution, and then mixing water and a water-soluble organic solvent. A method for producing a separator, comprising washing with a liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1077802A JP2734617B2 (en) | 1989-03-29 | 1989-03-29 | Manufacturing method of separator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1077802A JP2734617B2 (en) | 1989-03-29 | 1989-03-29 | Manufacturing method of separator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02256156A JPH02256156A (en) | 1990-10-16 |
| JP2734617B2 true JP2734617B2 (en) | 1998-04-02 |
Family
ID=13644139
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1077802A Expired - Fee Related JP2734617B2 (en) | 1989-03-29 | 1989-03-29 | Manufacturing method of separator |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2734617B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3324505B1 (en) | 2007-10-15 | 2023-06-07 | Ampt, Llc | Systems for highly efficient solar power |
-
1989
- 1989-03-29 JP JP1077802A patent/JP2734617B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02256156A (en) | 1990-10-16 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |