JP3160655B2 - Alkaline battery separator and manufacturing method thereof - Google Patents
Alkaline battery separator and manufacturing method thereofInfo
- Publication number
- JP3160655B2 JP3160655B2 JP30683692A JP30683692A JP3160655B2 JP 3160655 B2 JP3160655 B2 JP 3160655B2 JP 30683692 A JP30683692 A JP 30683692A JP 30683692 A JP30683692 A JP 30683692A JP 3160655 B2 JP3160655 B2 JP 3160655B2
- Authority
- JP
- Japan
- Prior art keywords
- separator
- fiber
- alkaline battery
- melamine
- nonwoven fabric
- 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
-
- 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
Landscapes
- Cell Separators (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明はＮｉ−Ｃｄ，Ｎｉ−Ｚ
ｎ，Ｎｉ−Ｈ電池等のアルカリ二次電池の高濃度アルカ
リ電解液に対し、優れた耐久性を有し、さらに吸液，保
液性能を増大させたアルカリ電池用セパレータおよびそ
の製造方法に関する。The present invention relates to Ni-Cd, Ni-Z
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a separator for an alkaline battery having excellent durability against a high-concentration alkaline electrolyte of an alkaline secondary battery such as an n, Ni-H battery, and further having improved liquid absorbing and retaining properties, and a method for producing the same.
【０００２】[0002]
【従来の技術】従来からアルカリ二次電池用セパレータ
に要求される特性として、電解液との親和性が良く、吸
液速度，保液性に優れる事、長期間の充放電の繰返し使
用に耐え得る耐アルカリ性，耐酸化性等の化学的安定性
に優れる事、内部抵抗が小さく、電極から発生するガス
の通過を妨げない通気性に優れる事等、種々の性能が要
求されている。2. Description of the Related Art Conventionally, the characteristics required for a separator for an alkaline secondary battery are that it has a good affinity for an electrolyte, has an excellent liquid absorption rate and liquid retention, and withstands repeated use of charge and discharge for a long time. Various performances are required, such as excellent chemical stability such as alkali resistance and oxidation resistance to be obtained, low internal resistance, and excellent air permeability that does not hinder the passage of gas generated from the electrodes.
【０００３】また、アルカリ二次電池用セパレータとし
ては従来よりポリアミド繊維の熱接着による不織布や、
ポリオレフィン系繊維の熱接着による不織布が用いられ
て来た。[0003] Further, as a separator for an alkaline secondary battery, a nonwoven fabric formed by heat bonding polyamide fibers,
Nonwoven fabrics formed by heat bonding of polyolefin fibers have been used.
【０００４】[0004]
【発明が解決しようとする課題】上記ポリアミド繊維か
らなる不織布は親水性に優れる為、電解液の吸液性，保
液性が高く、アルカリ電池用セパレータとして多用され
ているが、長期間の充放電の繰返し使用における化学的
耐久性に劣るという欠点があった。一方、高温度域にお
ける耐アルカリ性，耐酸化性等の化学的安定性に優れた
ポリプロピレン繊維、ポリエチレン繊維等のポリオレフ
ィン系繊維を用いた不織布から成るアルカリ電池用セパ
レータが種々提案されているが、オレフィン系繊維は親
水性に劣る為電解液保持性が極めて悪く、電解液がドラ
イアウトし易く急速充電，高率放電用途では使用出来な
いという欠点があった。The nonwoven fabric made of the above polyamide fiber is excellent in hydrophilicity, and therefore has a high liquid absorbing property and liquid retaining property of an electrolytic solution, and is frequently used as a separator for alkaline batteries. There is a disadvantage that the chemical durability in repeated use of discharge is poor. On the other hand, various types of alkaline battery separators made of nonwoven fabrics using polyolefin fibers such as polypropylene fiber and polyethylene fiber, which have excellent chemical stability such as alkali resistance and oxidation resistance in a high temperature range, have been proposed. Since the system fibers are inferior in hydrophilicity, they have extremely poor electrolyte retention properties, and have a drawback that the electrolyte is easily dried out and cannot be used for quick charge and high rate discharge applications.
【０００５】このため、従来からかかるポリオレフィン
系繊維に親水性を持たせるために、界面活性剤にて処理
する方法、繊維表面を発泡させる等凹凸を形成して表面
積を増大させる方法、プラズマ処理等により繊維表面を
活性化して電解液との親和性を向上させる方法、電子線
照射法により繊維表面に親水性モノマーをグラフト重合
させる方法、親水性を有するビニルアルコール等をオレ
フィンと共重合させた素材を適用する方法、スルホン化
処理等化学的後処理法により親水基を導入する方法等が
提案，検討されているが、いずれも長期間にわたる安定
な親水性を付与し、かつ連続して安定なものを得る事が
困難であるという問題があった。[0005] Therefore, in order to impart hydrophilicity to such polyolefin-based fibers, a method of treating the surface with a surfactant, a method of increasing the surface area by forming irregularities such as foaming the fiber surface, a plasma treatment, etc. A method of activating the fiber surface to improve the affinity with the electrolyte, a method of graft polymerizing a hydrophilic monomer to the fiber surface by electron beam irradiation, a material obtained by copolymerizing hydrophilic vinyl alcohol, etc. with an olefin A method of applying a hydrophilic group by a chemical post-treatment method such as a sulfonation treatment has been proposed and studied, but all of these methods provide a long-term stable hydrophilicity and are continuously stable. There was a problem that it was difficult to get things.
【０００６】したがって本発明の目的は、アルカリ電解
液との親和性に優れるとともに長期にわたる充放電の繰
返しに対しても安定なアルカリ電池用セパレータおよび
その製造方法を提供することである。Accordingly, an object of the present invention is to provide a separator for an alkaline battery which has excellent affinity with an alkaline electrolyte and is stable against repeated charging and discharging over a long period of time, and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】本発明は、耐薬品性繊維
から成る不織布シートの繊維交点および繊維表面の少な
くとも一部に付着したＮＢＲ（アクリロニトリル−ブタ
ジエン共重合ラバー）−メラミン架橋樹脂が、カルボキ
シル基およびスルホン酸基を有してなるものである。According to the present invention, there is provided a nonwoven fabric sheet made of a chemical resistant fiber, wherein the crosslinked resin of NBR (acrylonitrile-butadiene copolymer rubber) -melamine adhered to at least a part of the fiber intersection and at least part of the fiber surface is a carboxyl group. And a sulfonic acid group.
【０００８】本発明における耐薬品性繊維とは、ポリア
ミド繊維，ポリプロピレン（ＰＰ），ポリエチレン（Ｐ
Ｅ）等のポリオレフィン系繊維をいうが、これらの繊維
は単独で用いてもよく、また２種以上を併用してもよ
い。さらに、これらの繊維をたとえば、芯鞘構造等の複
合繊維として適宜混合使用してもよい。The chemical-resistant fiber in the present invention includes polyamide fiber, polypropylene (PP) and polyethylene (P).
The fibers refer to polyolefin fibers such as E), and these fibers may be used alone or in combination of two or more. Further, these fibers may be appropriately mixed and used, for example, as a composite fiber having a core-sheath structure or the like.
【０００９】本発明に用いるＮＢＲ−メラミン架橋樹脂
とは、ＮＢＲ樹脂にトリメチロールメラミン，ヘキサメ
チロールメラミン，メトキシ化トリメチロールメラミン
等のメラミン系樹脂を架橋し、耐水性，耐薬品性を向上
させたものをいう。上記ＮＢＲ−メラミン架橋樹脂は、
ディッピング，コーティング，発泡コーティング等の手
法により、不織布シートに被覆する事が可能であり、特
に限定されるものではないが、良好なる電解液親和性及
び浸透性，保液性を付与する為には発泡コーティング法
による事が特に好ましい。The NBR-melamine cross-linked resin used in the present invention is obtained by cross-linking an NBR resin with a melamine resin such as trimethylol melamine, hexamethylol melamine, or methoxylated trimethylol melamine to improve water resistance and chemical resistance. A thing. The NBR-melamine cross-linked resin,
It is possible to coat the non-woven fabric sheet by a technique such as dipping, coating, foam coating, etc., but it is not particularly limited, but in order to provide good electrolyte affinity, permeability and liquid retention. It is particularly preferable to use the foam coating method.
【００１０】また本発明は、耐薬品性繊維に対するＮＢ
Ｒ−メラミン架橋樹脂の付着割合が３〜５０重量％であ
ることを特徴とする。[0010] The present invention also relates to an NB for chemical resistant fibers.
The R-melamine crosslinked resin has an adhesion ratio of 3 to 50% by weight.
【００１１】上記付着割合が３重量％未満では、電解液
との親和性の向上が見られず、５０重量％を超えるとア
ルカリ電池用セパレータに要求される通気性が阻害さ
れ、好ましくない。When the adhesion ratio is less than 3% by weight, no improvement in affinity with the electrolyte is observed, and when it exceeds 50% by weight, the air permeability required for an alkaline battery separator is impaired, which is not preferable.
【００１２】ところで、上記ＮＢＲ−メラミン架橋樹脂
は、アクリロニトリルの含有量が多い程、親水性，耐薬
品性に安定なものとなる反面、樹脂が硬化して脆い性質
となる。このため、カルボキシル基導入時の加水分解の
後の強度低下をきたすことから、５０重量％以下の含有
量であることが望ましい。また、アクリロニトリルの含
有量が１０重量％未満になると、親水性，耐薬品性の低
下が著しいため、１０重量％以上であることが望まし
い。By the way, the NBR-melamine crosslinked resin becomes more hydrophilic and more chemically resistant as the content of acrylonitrile increases, but the resin hardens and becomes brittle. For this reason, it is desirable that the content is 50% by weight or less, since the strength is reduced after hydrolysis at the time of introducing a carboxyl group. When the content of acrylonitrile is less than 10% by weight, hydrophilicity and chemical resistance are remarkably reduced, so that the content is preferably 10% by weight or more.
【００１３】また本発明は、耐薬品性繊維から成る不織
布シートに、ＮＢＲ−メラミン架橋樹脂を含む結合剤を
付着させた後、加水分解処理，スルホン化処理をこの順
序で行なうものである。Further, in the present invention, after a binder containing an NBR-melamine crosslinked resin is adhered to a nonwoven fabric sheet made of a chemical resistant fiber, a hydrolysis treatment and a sulfonation treatment are performed in this order.
【００１４】上記加水分解処理とは、ＮＢＲ−メラミン
架橋樹脂中のニトリル基（−ＣＮ）を、アルカリ処理等
による加水分解により親水基であるカルボキシル基（−
ＣＯＯＨ）に変成させるものである。この反応は、下記
一般式に示すように二段階で進行し、ＮＢＲ−メラミン
架橋樹脂にカルボキシル基が導入される。The above-mentioned hydrolysis treatment means that the nitrile group (-CN) in the NBR-melamine crosslinked resin is converted into a carboxyl group (-
COOH). This reaction proceeds in two steps as shown in the following general formula, and a carboxyl group is introduced into the NBR-melamine crosslinked resin.
【００１５】[0015]
【化１】 Embedded image
【００１６】また、上記スルホン化処理とは、ＳＯ3 ガ
ス、発煙硫酸、高濃度の濃硫酸等による公知の方法で行
なうものであり、下記に示すように、加水分解処理され
たＮＢＲ−メラミン架橋樹脂のカルボキシル基が結合し
た３級炭素原子に、親水基であるスルホン酸基（−ＳＯ
3 Ｈ）が導入される。The above-mentioned sulfonation treatment is carried out by a known method using SO 3 gas, fuming sulfuric acid, high-concentration sulfuric acid, etc., as described below. A tertiary carbon atom to which a carboxyl group of the resin is bonded is attached to a sulfonic acid group (-SO
3 H) is introduced.
【００１７】[0017]
【化２】 Embedded image
【００１８】[0018]
【作用】本発明に従えば、親水性を有するカルボキシル
基およびスルホン酸基が導入されたＮＢＲ−メラミン架
橋樹脂によって、不織布シートは親水性に優れたものと
なり、これによって長期間にわたる電解液親和性，保液
性に優れるとともに長期間にわたる充放電の繰返しに対
しても安定なアルカリ電池用セパレータを得ることがで
きる。According to the present invention, the NBR-melamine cross-linked resin having a carboxyl group and a sulfonic acid group having hydrophilicity makes the nonwoven fabric sheet excellent in hydrophilicity, thereby having a long-term compatibility with the electrolyte for a long time. In addition, it is possible to obtain a separator for an alkaline battery which has excellent liquid retention properties and is stable against repeated charging and discharging over a long period of time.
【００１９】[0019]
【実施例】以下、実施例により本発明をさらに具体的に
説明する。The present invention will be described more specifically with reference to the following examples.
【００２０】（実施例）芯がポリプロピレン、鞘がポリ
エチレンにより構成される芯鞘型加熱接着性繊維（０．
９ｄ×３８ｍｍ）３０％と、レギュラーのポリプロピレ
ン繊維（１．５ｄ×３８ｍｍ）７０％との混合繊維より
なるウエブを、１３０℃に加熱した一対のカレンダーロ
ールで加熱圧着し、目付６５ｇ／ｍ2 、厚さ０．２０ｍ
ｍの不織布シートＡを得た。(Embodiment) A core-sheath type heat-adhesive fiber having a core made of polypropylene and a sheath made of polyethylene (0.
A web made of a mixed fiber of 30% of 9d × 38 mm) and 70% of regular polypropylene fiber (1.5d × 38 mm) is heat-pressed with a pair of calender rolls heated to 130 ° C., and has a basis weight of 65 g / m 2 . 0.20m thick
m of the nonwoven fabric sheet A was obtained.
【００２１】次に、アクリロニトリルの含有量が３５重
量％であるＮＢＲ樹脂１００重量部に対し、トリメチロ
ールメラミン３５重量部及びアミン系の硬化触媒３重量
部を配合した結合材を、発泡コーティング法により上記
不織布シートＡに均一に含浸後、乾燥，熱処理加工し
て、目付７１ｇ／ｍ2 の不織布シートＢを形成した。Next, a binder prepared by blending 35 parts by weight of trimethylolmelamine and 3 parts by weight of an amine-based curing catalyst with 100 parts by weight of an NBR resin having an acrylonitrile content of 35% by weight was subjected to a foam coating method. The nonwoven sheet A was uniformly impregnated, dried and heat-treated to form a nonwoven sheet B having a basis weight of 71 g / m 2 .
【００２２】さらに該不織布シートＢを、１０％ＫＯＨ
溶液中にて９５℃、３０分間の条件により加水分解処理
し、その後洗浄処理を実施した後乾燥して、引続き該不
織布シートをＳＯ3 ガス濃度が８Ｖｏｌ％、温度６０℃
のガス雰囲気中で３０秒間の気層接触処理を行なった
後、水洗，希アンモニア水による中和処理を経て、さら
に十分に洗浄後乾燥して本実施例のアルカリ電池用セパ
レータを得た。Further, the nonwoven fabric sheet B is
The solution is hydrolyzed at 95 ° C. for 30 minutes in a solution, then washed and dried, and then the nonwoven fabric sheet is subjected to a SO 3 gas concentration of 8 vol% and a temperature of 60 ° C.
After performing a gas layer contact treatment for 30 seconds in the above gas atmosphere, the substrate was washed with water, neutralized with dilute aqueous ammonia, further sufficiently washed, and dried to obtain a separator for an alkaline battery of this example.
【００２３】（比較例１）上記実施例で得た不織布シー
トＡを比較例１のアルカリ電池用セパレータとした。Comparative Example 1 The nonwoven fabric sheet A obtained in the above example was used as the alkaline battery separator of Comparative Example 1.
【００２４】（比較例２）上記実施例で得た不織布シー
トＢを比較例２のアルカリ電池用セパレータとした。Comparative Example 2 The nonwoven fabric sheet B obtained in the above example was used as a separator for an alkaline battery of Comparative Example 2.
【００２５】（比較例３）６−ナイロン繊維（１．５ｄ
×３８ｍｍ）７０％と、芯部が６−ナイロン、鞘部が融
点１６０℃のナイロン６−１０−１２の三元共重合体で
なる芯鞘型熱融着繊維（２ｄ×３８ｍｍ）３０％との混
合繊維よりなるウエブを、１６０℃に加熱した一対のカ
レンダーロールで加熱圧着して得た目付８０ｇ／ｍ2 、
厚さ０．２０ｍｍの不織布シートを比較例３のアルカリ
電池用セパレータとした。(Comparative Example 3) 6-nylon fiber (1.5 d
× 38 mm) 70%, and 30% of a core-sheath type heat-fused fiber (2d × 38 mm) composed of a 6-nylon core and a terpolymer of nylon 6-10-12 having a melting point of 160 ° C. Of a mixed fiber heated and compressed by a pair of calender rolls heated to 160 ° C., and a basis weight of 80 g / m 2 ,
A nonwoven fabric sheet having a thickness of 0.20 mm was used as the separator for an alkaline battery of Comparative Example 3.
【００２６】以下、実施例および比較例１〜３で得たア
ルカリ電池用セパレータの諸物性の比較テストを行なっ
た結果を表１に示す。Table 1 shows the results of comparative tests of various physical properties of the alkaline battery separators obtained in the examples and comparative examples 1 to 3.
【００２７】[0027]
【表１】 [Table 1]
【００２８】表中、試験項目のテスト方法は下記の通り
である。 吸液速度 ；比重１．３０の苛性カリ溶液中に試料巾
２５ｍｍのセパレータ材の一端を浸漬、３０分後の吸液
高さ。 保液率 ；比重１．３０の苛性カリ溶液中にセパレ
ータ材を浸漬し、１０分間吊り干し、水切り後の溶液吸
収率。 耐アルカリ性；比重１．３０の苛性カリ溶液中に８０℃
にて３０日間浸漬した時の重量減少率。 耐酸化性試験後強度保持率；５％ＫＭｎＯ4 溶液２５０
ｍｌと、比重１．３０の苛性カリ溶液５０ｍｌとの混合
液中で５０℃，１時間浸漬した後のセパレータ引張強力
保持率。In the table, the test methods of the test items are as follows. Liquid absorption speed; One end of a separator material having a sample width of 25 mm was immersed in a caustic potassium solution having a specific gravity of 1.30, and the liquid absorption height after 30 minutes. Liquid retention ratio: The separator material was immersed in a caustic potassium solution having a specific gravity of 1.30, hung up for 10 minutes, and drained to remove the solution. Alkali resistance; 80 ° C in caustic potassium solution with specific gravity of 1.30
The weight loss rate when immersed for 30 days. Strength retention after oxidation resistance test: 5% KMnO 4 solution 250
The tensile strength retention of the separator after immersion at 50 ° C. for 1 hour in a mixed solution of 50 ml of a potassium hydroxide solution having a specific gravity of 1.30 and a specific gravity of 1.30.
【００２９】上記表１より明らかなように、本実施例に
よるセパレータは、優れた電解液親和性を示し、比較例
３のナイロン繊維を用いたセパレータに匹敵する吸液
性，保液性を有する事が窺われる。また、耐アルカリ
性，耐酸化性に於いても良好なる耐久性を有し、本実施
例によるアルカリ電池用セパレータを電池に組み込み、
充放電を繰返し行なっても長期間にわたる使用に十分耐
えることを示す。As is evident from Table 1, the separator according to the present example has excellent electrolyte affinity and has a liquid absorbing property and a liquid retaining property comparable to the separator using the nylon fiber of Comparative Example 3. Things are seen. In addition, it has good durability in terms of alkali resistance and oxidation resistance, and the alkaline battery separator according to the present embodiment is incorporated in a battery.
It shows that it can withstand long-term use even after repeated charging and discharging.
【００３０】[0030]
【発明の効果】本発明は上記の如く構成した事により、
長期にわたり電解液との親和性を維持出来るとともに、
更に良好なる耐久性を有する為、長期間にわたる充放電
の繰返しに対しても安定であり、電池寿命を大巾に改善
することが可能なアルカリ電池用セパレータを得ること
ができる。According to the present invention having the above-described structure,
While maintaining the affinity with the electrolyte for a long time,
Further, since the battery has good durability, it is stable against repeated charge and discharge over a long period of time, and an alkaline battery separator capable of greatly improving the battery life can be obtained.
Claims (3)
維交点および繊維表面の少なくとも一部に付着したＮＢ
Ｒ（アクリロニトリル−ブタジエン共重合ラバー）−メ
ラミン架橋樹脂が、カルボキシル基およびスルホン酸基
を有してなることを特徴とするアルカリ電池用セパレー
タ。An NB attached to at least a part of a fiber intersection and a fiber surface of a nonwoven fabric sheet made of a chemical resistant fiber.
A separator for an alkaline battery, wherein R (acrylonitrile-butadiene copolymer rubber) -melamine crosslinked resin has a carboxyl group and a sulfonic acid group.
基およびスルホン酸基を有するＮＢＲ−メラミン架橋樹
脂の付着割合が、３〜５０重量％である請求項１記載の
アルカリ電池用セパレータ。2. The alkaline battery separator according to claim 1, wherein the adhesion ratio of the NBR-melamine crosslinked resin having a carboxyl group and a sulfonic acid group to the chemical resistant fiber is 3 to 50% by weight.
ＢＲ−メラミン架橋樹脂を含む結合剤を付着させた後、
加水分解処理、スルホン化処理をこの順序で行なうこと
を特徴とするアルカリ電池用セパレータの製造方法。3. A nonwoven fabric sheet made of a chemical-resistant fiber,
After attaching a binder comprising a BR-melamine cross-linked resin,
A method for producing a separator for an alkaline battery, comprising performing a hydrolysis treatment and a sulfonation treatment in this order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30683692A JP3160655B2 (en) | 1992-11-17 | 1992-11-17 | Alkaline battery separator and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30683692A JP3160655B2 (en) | 1992-11-17 | 1992-11-17 | Alkaline battery separator and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06163020A JPH06163020A (en) | 1994-06-10 |
| JP3160655B2 true JP3160655B2 (en) | 2001-04-25 |
Family
ID=17961845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30683692A Expired - Fee Related JP3160655B2 (en) | 1992-11-17 | 1992-11-17 | Alkaline battery separator and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3160655B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3437448B2 (en) * | 1998-06-09 | 2003-08-18 | 株式会社ユアサコーポレーション | Sealed battery separator |
| JP2002216566A (en) * | 2001-01-22 | 2002-08-02 | Sony Corp | Submerged electric switch and its manufacturing method |
| CN113161549B (en) * | 2021-03-25 | 2022-08-02 | 万向一二三股份公司 | Photo-crosslinking binder system, slurry composition containing photo-crosslinking binder system and application of slurry composition |
-
1992
- 1992-11-17 JP JP30683692A patent/JP3160655B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06163020A (en) | 1994-06-10 |
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| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |