JPH039931A - Preparation of water-absorbing polyamide fiber, film and sheet - Google Patents

Preparation of water-absorbing polyamide fiber, film and sheet

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Publication number
JPH039931A
JPH039931A JP14308889A JP14308889A JPH039931A JP H039931 A JPH039931 A JP H039931A JP 14308889 A JP14308889 A JP 14308889A JP 14308889 A JP14308889 A JP 14308889A JP H039931 A JPH039931 A JP H039931A
Authority
JP
Japan
Prior art keywords
water
polyamide
film
solvent
salt
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.)
Pending
Application number
JP14308889A
Other languages
Japanese (ja)
Inventor
Yasufumi Miyawaki
宮脇 康文
Kunio Kondo
近土 邦雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Asahi Chemical Industry Co Ltd
Original Assignee
Asahi Chemical Industry Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Asahi Chemical Industry Co Ltd filed Critical Asahi Chemical Industry Co Ltd
Priority to JP14308889A priority Critical patent/JPH039931A/en
Publication of JPH039931A publication Critical patent/JPH039931A/en
Pending legal-status Critical Current

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  • Artificial Filaments (AREA)

Abstract

PURPOSE:To obtain polyamide fiber, film and sheet with high water absorption and water retention by dissolving a polyamide in an amide solvent by heating, molding it and removing the solvent after cooling and gelation. CONSTITUTION:A polyamide is dissolved in an amide solvent along optionally contg. an inorg. salt by heating and the soln. is extruded from a spinneret or cast on a plane. After cooling and gelation, the solvent and the salt are removed in one or more steps. The mol.wt. of the polyamide used is usually approximately 15,000-500,000. Examples of the amide solvent include N-methyl-2- pyrrolidone and N,N-dimenthylacetamide. As the inorg. salt, lithium chloride and calcium chloride are used. The water absorbing polyamide fiber, film and sheet mostly exhibit a water absorption of approximately 1,200-1,500% and a water retention after centrifugal dehydration of about 800% which depend a little on the manufacturing conditions.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は吸水性ポリアミド繊維、フィルム、シートの製
造法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing water-absorbing polyamide fibers, films, and sheets.

〔従来の技術〕[Conventional technology]

水を吸収する材料として古くから、脱脂綿、バルブ、木
綿布などが用いられてきた。これらの材料は、毛細管現
象により基材の間隙に水を吸収するのみで吸水力は低く
、圧力をかけることにより、簡単に水を吐き出してしま
うものである。又、−般に衣料用に用いられ吸水性の繊
維であるレーヨン、綿、羊毛では、吸水率はどれも80
0%程度であり、遠心脱水によるこれらの保水率はそれ
ぞれ100%、50%、133%程度である。ポリアミ
ドでも、従来よりよく用いられているナイロンでは遠心
脱水による保水率は14%と非常に低い値を示す。
Absorbent cotton, bulbs, and cotton cloth have long been used as materials to absorb water. These materials only absorb water into the gaps in the base material due to capillary action, and have low water absorption power, and water is easily expelled by applying pressure. Also, - Rayon, cotton, and wool, which are water-absorbent fibers commonly used for clothing, all have a water absorption rate of 80%.
The water retention rates obtained by centrifugal dehydration are approximately 100%, 50%, and 133%, respectively. Among polyamides, nylon, which has been commonly used in the past, exhibits a very low water retention rate of 14% when subjected to centrifugal dehydration.

衣料用、農業・園芸用の保水シート等では吸水率が高く
、更に保水率も高い素材が要望されているが、従来のレ
ーヨン、綿、羊毛、特に一般のナイロンでは保水率が極
めて低くこの要望を満たすことができていない。
There is a demand for materials with high water absorption and even high water retention rates for water retention sheets for clothing, agriculture and gardening, etc. However, conventional rayon, cotton, wool, and especially ordinary nylon have extremely low water retention rates, and this demand cannot be met. have not been able to meet the requirements.

〔発明が解決しようとする課題〕[Problem to be solved by the invention]

本発明の目的は、上述の問題を解決し、吸水率が高く、
更に保水率も高いポリアミド繊維、フィルム、シート素
材を提供することにある。
The purpose of the present invention is to solve the above-mentioned problems, have high water absorption rate,
Another object of the present invention is to provide polyamide fibers, films, and sheet materials that have a high water retention rate.

〔課題を解決する為の手段] 本発明は、ポリアミドをアミド型溶剤単体もしくは無機
塩を含むアミド型溶剤に加熱溶解し、これを紡糸口金よ
り押し出すか、又は平面上にキャストし、冷却ゲル化後
、溶剤及び塩を一段もしくは多段階的に除去することを
特徴とする吸水性ポリアミド繊維、フィルム、シートの
製造法、である。
[Means for Solving the Problems] The present invention involves heating and dissolving polyamide in an amide type solvent alone or an amide type solvent containing an inorganic salt, extruding it from a spinneret or casting it on a flat surface, and cooling and gelling it. After that, the solvent and salt are removed in one step or in multiple steps.

本発明に用いられるポリアミドはナイロン6、ナイロン
66等の脂肪族ポリアミド及び、ポリメタフェニレンイ
ソフタルアミド1、ポリパラフェニレンテレフタルアミ
ド等の芳香族ポリアミド等であり、用いられるアミド型
溶剤は特に限定するものではないが、N−メチル−2−
ピロリドン、1.3−ジメチルイミダゾリジノン、N、
N−ジメチルアセトアミド等である。又、混合して用い
られる無機塩は塩化リチウム、塩化カルシウムである。
The polyamides used in the present invention include aliphatic polyamides such as nylon 6 and nylon 66, and aromatic polyamides such as polymetaphenylene isophthalamide 1 and polyparaphenylene terephthalamide, and the amide type solvent used is not particularly limited. but not N-methyl-2-
pyrrolidone, 1,3-dimethylimidazolidinone, N,
N-dimethylacetamide and the like. In addition, the inorganic salts used in combination are lithium chloride and calcium chloride.

以下に製造過程にそうで詳細に説明する。The manufacturing process will be explained in detail below.

まずポリアミドをアミド型溶剤単体、もしくは無機塩を
含むアミド型溶剤に加熱溶解する。この際、ポリマー濃
度は任意であるが一般には1重量%から30重量%が用
いられる。又、溶解温度は、ポリマーが溶剤系に溶解す
る温度以上からポリマーの分解温度以下の範囲で任意で
あるが、−aには130〜220°Cが用いられ、より
好ましくは150〜200°Cである。この温度より高
いと、溶剤系に含まれる若干量の水分等でポリマーの加
水分解が起こる可能性がある。溶解温度を下げるために
、無機塩として塩化リチウム、塩化カルシウムが用いら
れる。これらは量的には任意であるが、一般には1重量
%から50重量%が好ましい。
First, polyamide is heated and dissolved in an amide type solvent alone or an amide type solvent containing an inorganic salt. At this time, the polymer concentration is arbitrary, but generally 1% to 30% by weight is used. Further, the dissolution temperature is arbitrary in the range from the temperature at which the polymer dissolves in the solvent system to the decomposition temperature of the polymer, but -a is preferably 130 to 220°C, more preferably 150 to 200°C. It is. If the temperature is higher than this, hydrolysis of the polymer may occur due to a small amount of water contained in the solvent system. In order to lower the dissolution temperature, lithium chloride and calcium chloride are used as inorganic salts. Although the amount of these components is arbitrary, it is generally preferred to range from 1% by weight to 50% by weight.

又、無機塩は単体であっても、2種の混合物であっても
構わない。
Further, the inorganic salt may be used alone or in a mixture of two types.

ポリマーの分子量は特に限定するものではないが、一般
に1,5万〜50万のものが用いられる。
Although the molecular weight of the polymer is not particularly limited, a molecular weight of 1,50,000 to 500,000 is generally used.

ポリアミド繊維、フィルム、シートフィルム、シートの
強度を上げようとするならば、比較的高重合度のものを
用いれば良い。なお、分子量10万以上の高分子量ポリ
アミドは、以下のようにして製造できる。詳しくは、特
願昭63−113491号に記載された方法に準拠して
製造すれば良い。
If it is desired to increase the strength of polyamide fibers, films, and sheets, polyamide fibers, films, and sheets having a relatively high degree of polymerization may be used. Note that a high molecular weight polyamide having a molecular weight of 100,000 or more can be produced as follows. Specifically, it may be manufactured according to the method described in Japanese Patent Application No. 113491/1983.

まず、溶融重合などにより、分子量が1万〜2万で、か
つ末端カルボキシル基濃度と末端アミド基濃度との差が
−15〜+ 15 mgeq/kg、かつ末端アミド基
濃度と末端カルボキシル基濃度との比が0.6<([−
NHz] / [−COOII] )d、1であるプレ
ポリマーを製造する0両末端基部度差及び比をこの範囲
になるようにするには、モノマー(ジアミンとジカルボ
ン酸)の仕込み量比の調節や重合条件の調節などで行う
First, by melt polymerization etc., the molecular weight is 10,000 to 20,000, the difference between the terminal carboxyl group concentration and the terminal amide group concentration is -15 to +15 mgeq/kg, and the terminal amide group concentration and the terminal carboxyl group concentration are The ratio of 0.6<([-
NHz] / [-COOII] ) d, 0 to produce a prepolymer that is 1. In order to keep the difference and ratio of both end groups within this range, adjust the ratio of the monomers (diamine and dicarboxylic acid) to be charged. This is done by adjusting the polymerization conditions.

このプレポリマーの製造時に、次亜燐酸ソーダなどの重
合触媒を添加することが好ましい。
It is preferable to add a polymerization catalyst such as sodium hypophosphite during the production of this prepolymer.

次に、得られたプレポリマーを、そのポリマーの融点に
近い温度で、例えばナイロン66では200〜240℃
の温度で面相重合する。固相重合においては、真空下ま
たは窒素などの不活性ガス中で行う。
The resulting prepolymer is then heated at a temperature close to the melting point of the polymer, e.g. 200-240°C for nylon 66.
It undergoes surface phase polymerization at a temperature of . In solid phase polymerization, it is carried out under vacuum or in an inert gas such as nitrogen.

次に、上述のようにして得られたポリマー溶液を紡糸口
金より押し出して繊維状にするか、又は平面上にキャス
トしてフィルム、シート状に成形する。これらを冷却ゲ
ル化させる。この際の冷却温度は、ポリマー分子量、ポ
リマー濃度、無機塩濃度により変化する。一般には室温
から一10℃付近が使用しやすい。
Next, the polymer solution obtained as described above is extruded from a spinneret to form a fiber, or cast onto a flat surface to form a film or sheet. These are cooled and gelled. The cooling temperature at this time varies depending on the polymer molecular weight, polymer concentration, and inorganic salt concentration. Generally, temperatures between room temperature and around -10°C are easy to use.

続いて得られたゲル化繊維、フィルム、シートより溶剤
及び塩を一段もしくは多段階的に除去することにより、
吸水性のあるポリアミド繊維、フィルム、シートが製造
される。抽出により溶剤、塩を除去した場合は、乾燥に
より抽出溶媒を除去してやれば良い、用いられる抽出剤
は、溶剤及び塩を溶解し、ポリマーを溶解しないもので
あればなんでもよく、例えば、メタノール、エタノール
、アセトン、酢酸エチル等が用いられる。
By subsequently removing the solvent and salt from the resulting gelled fibers, films, and sheets in one or multiple steps,
Water absorbent polyamide fibers, films and sheets are produced. When the solvent and salt are removed by extraction, the extraction solvent can be removed by drying.The extractant used may be any one that dissolves the solvent and salt but does not dissolve the polymer.For example, methanol, ethanol, etc. , acetone, ethyl acetate, etc. are used.

得られる吸水性ポリアミド繊維、フィルム、シートは白
色をしており、成形体内には約1μm〜2μm程度の孔
があり、網目状を呈している。
The resulting water-absorbing polyamide fibers, films, and sheets are white in color, and have pores of about 1 μm to 2 μm in the molded body, giving them a mesh-like appearance.

得られる吸水性ポリアミド繊維、フィルム、シートは製
造条件により多少の差はあるがほとんどのものが吸水率
で約1200〜1500%を示し、遠心脱水した後も約
800%の保水率を示すものである。
The resulting water-absorbent polyamide fibers, films, and sheets have a water absorption rate of about 1200 to 1500%, although there are some differences depending on the manufacturing conditions, and even after centrifugal dehydration, they show a water retention rate of about 800%. be.

本発明により得られるポリアミド繊維、フィルム、シー
トが良好な吸水性、保水性を示すのは、元来、水が吸着
しゃすいアミドであること、さらに水の入るスペースと
して多孔質であること、又、分子量の高いポリマーを用
いることにより繊維、フィルム、シートの強度が上がり
、潰れにく(なるため、圧力による離水が少なくなるも
のであると考えられる。
The reason why the polyamide fibers, films, and sheets obtained by the present invention exhibit good water absorption and water retention properties is that they are inherently water-absorbing amides, and that they are porous as spaces for water to enter. It is thought that by using a polymer with a high molecular weight, the strength of fibers, films, and sheets increases and they become less likely to collapse (thus, water separation due to pressure is reduced).

〔実施例〕〔Example〕

以下、実施例により本発明をさらに詳細に説明する。 Hereinafter, the present invention will be explained in more detail with reference to Examples.

ここで言う吸水率とは減圧乾燥(室温、12時間)によ
り乾燥したポリアミド繊維、フィルム、シートの重量を
測定(A)シ、これらを水に5分間浸漬吸水させた後取
り出して表面の水分を拭き取り重量を測定(B)シ、吸
水率−(B−A) /Ax100(%)で計算したもの
であり、保水率とは吸水したポリアミド繊維、フィルム
、シートを、遠心脱水機により3000rpmで5分間
脱水した後、重量を測定(C)シ、保水率=(C−A)
/Ax100(%)で計算したものである。
The water absorption rate referred to here refers to the weight of polyamide fibers, films, and sheets that have been dried under reduced pressure (room temperature, 12 hours). (A) After immersing them in water for 5 minutes to absorb water, take them out and remove the moisture on the surface. The wiped weight was measured (B), and it was calculated as water absorption rate - (B-A) /Ax100 (%). After dehydrating for a minute, measure the weight (C), water retention rate = (C-A)
/Ax100 (%).

実施例1 冷却管、ヘリカル状撹拌翼を備えた300dのセパラブ
ルフラスコに分子量2万のナイロン66を40.OOg
、塩化リチウム15.04g、 N−メチル−2−ピロ
リドン200dを仕込み、165°Cにて加熱溶解した
。得られたポリマー溶液を室温の81角のガラス板上に
流延し、その温度で冷却後、酢酸エチル250m、続い
てメタノール250dで溶剤を抽出し、室温で減圧乾燥
して厚さ280μmのポリアミドフィルムを得た。これ
を水浴に5分間浸漬した後、水浴より取りだし、表面に
ついた水滴を拭きとり重量測定により吸水率を計算した
ところ吸水率は1350%であった。この吸水したフィ
ルムを遠心脱水機により3000rpmで5分間脱水し
た後、重量測定により保水率を計算したところ保水率は
800%であった。
Example 1 Nylon 66 with a molecular weight of 20,000 was placed in a 300 d separable flask equipped with a cooling tube and a helical stirring blade. OOg
, 15.04 g of lithium chloride, and 200 d of N-methyl-2-pyrrolidone were charged and dissolved by heating at 165°C. The obtained polymer solution was cast onto an 81 square glass plate at room temperature, and after cooling at that temperature, the solvent was extracted with 250 m of ethyl acetate, followed by 250 m of methanol, and dried under reduced pressure at room temperature to form a polyamide with a thickness of 280 μm. Got the film. After immersing this in a water bath for 5 minutes, it was taken out from the water bath, water droplets adhering to the surface were wiped off, and the water absorption rate was calculated by weight measurement, and the water absorption rate was 1350%. After the water-absorbed film was dehydrated for 5 minutes at 3000 rpm using a centrifugal dehydrator, the water retention rate was calculated by weight measurement and was found to be 800%.

実施例2 実施例1の分子量2万のナイロン66 40.OOgを
分子量15万のナイロン66 14.OOgに、塩化リ
チウム15.04 gを塩化リチウム5.27gに変え
た以外は実施例1と同様にポリアミドフィルムを作成し
た。厚さは260μmのポリアミドフィルムとなった。
Example 2 Nylon 66 of Example 1 with a molecular weight of 20,000 40. OOg as nylon 66 with a molecular weight of 150,000 14. A polyamide film was prepared in the same manner as in Example 1 except that 15.04 g of lithium chloride was changed to 5.27 g of lithium chloride. The resulting polyamide film had a thickness of 260 μm.

これを実施例1と同様にして吸水率、保水率を調べたと
ころ、それぞれ1450%、820%あった。
When the water absorption rate and water retention rate were examined in the same manner as in Example 1, they were 1450% and 820%, respectively.

実施例3 実施例1と同様にポリマー溶液を調製した後、これを0
.5 mm−の紡糸口金より空気中に押し出し、酢酸エ
チル浴、続いてメタノール浴を通し、乾燥して繊維径0
.48mmφのポリアミド繊維を得た。
Example 3 After preparing a polymer solution in the same manner as in Example 1, it was
.. The fibers were extruded into air through a 5 mm spinneret, passed through an ethyl acetate bath, then a methanol bath, and dried until the fiber diameter was 0.
.. Polyamide fibers with a diameter of 48 mm were obtained.

これを実施例1と同様にして吸水率、保水率を調べたと
ころ、それぞれ1300%、850%であった。
The water absorption rate and water retention rate were examined in the same manner as in Example 1 and found to be 1300% and 850%, respectively.

比較例 分子量3万のナイロン66ポリマーを溶融し、0、2 
armφの紡糸口金より空気中に押し出し、冷却して繊
維径0.07 tmφのポリアミド繊維を得た。
Comparative Example A nylon 66 polymer with a molecular weight of 30,000 was melted and
It was extruded into the air through an armφ spinneret and cooled to obtain polyamide fibers with a fiber diameter of 0.07 tmφ.

これを実施例1と同様にして吸水率、保水率を調べたと
ころ、それぞれ100%、20%であった。
When the water absorption rate and water retention rate were examined in the same manner as in Example 1, they were 100% and 20%, respectively.

以下 余白 〔発明の効果] 本発明によれば、吸水率、保水率の高い吸水性ポリアミ
ド繊維、フィルム、シートを製造することができる。
Margin [Effects of the Invention] According to the present invention, water-absorbing polyamide fibers, films, and sheets with high water absorption and water retention can be produced.

本発明により得られる吸水性ポリアミド繊維、フィルム
、シートは、衣料分野、農業・園芸用の保水シート分野
等の吸水要求性能を満たす種々の方面に利用されるもの
である。
The water-absorbing polyamide fibers, films, and sheets obtained according to the present invention are used in various fields that meet water absorption performance requirements, such as the field of clothing and the field of water-retaining sheets for agriculture and horticulture.

Claims (1)

【特許請求の範囲】[Claims] 1、ポリアミドをアミド型溶剤単体もしくは無機塩を含
むアミド型溶剤に加熱溶解し、これを紡糸口金より押し
出すか、又は平面上にキャストし、冷却ゲル化後、溶剤
及び塩を一段もしくは多段階的に除去することを特徴と
する吸水性ポリアミド繊維、フィルム、シートの製造法
1. Polyamide is heated and dissolved in an amide type solvent alone or an amide type solvent containing an inorganic salt, extruded from a spinneret or cast on a flat surface, cooled and gelled, and then the solvent and salt are added in one or multiple steps. A method for producing water-absorbing polyamide fibers, films, and sheets, which is characterized by removing water.
JP14308889A 1989-06-07 1989-06-07 Preparation of water-absorbing polyamide fiber, film and sheet Pending JPH039931A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP14308889A JPH039931A (en) 1989-06-07 1989-06-07 Preparation of water-absorbing polyamide fiber, film and sheet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP14308889A JPH039931A (en) 1989-06-07 1989-06-07 Preparation of water-absorbing polyamide fiber, film and sheet

Publications (1)

Publication Number Publication Date
JPH039931A true JPH039931A (en) 1991-01-17

Family

ID=15330633

Family Applications (1)

Application Number Title Priority Date Filing Date
JP14308889A Pending JPH039931A (en) 1989-06-07 1989-06-07 Preparation of water-absorbing polyamide fiber, film and sheet

Country Status (1)

Country Link
JP (1) JPH039931A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995031499A1 (en) * 1994-05-18 1995-11-23 Asahi Kasei Kogyo Kabushiki Kaisha Ion-conductive film and precursor film therefor
EP0722987A1 (en) * 1995-01-17 1996-07-24 Teijin Limited Polyamide solution composition and methods for producing fibrids and paper-like sheets using the same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995031499A1 (en) * 1994-05-18 1995-11-23 Asahi Kasei Kogyo Kabushiki Kaisha Ion-conductive film and precursor film therefor
US5834112A (en) * 1994-05-18 1998-11-10 Asahi Kasei Kogyo Kabushiki Kaisha Ion conductive film and precursor film thereof
EP0722987A1 (en) * 1995-01-17 1996-07-24 Teijin Limited Polyamide solution composition and methods for producing fibrids and paper-like sheets using the same
US5723568A (en) * 1995-01-17 1998-03-03 Teijin Limited Polyamide solution composition and methods for producing fibrids and paper-like sheets using the same

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