JP2016017230A - Method for producing acrylic fiber bundle - Google Patents
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Abstract
Description
本発明は、アクリル繊維束の製造方法に関する。更に詳しくは、溶剤を含む凝固繊維束の溶剤を効率良く脱溶剤するための洗浄する工程を有するアクリル繊維束の製造方法に関する。 The present invention relates to a method for producing an acrylic fiber bundle. More specifically, the present invention relates to a method for producing an acrylic fiber bundle having a cleaning step for efficiently removing the solvent of the coagulated fiber bundle containing the solvent.
一般にアクリル繊維の製造工程では重合体が溶剤に溶解した重合体溶液を紡糸ノズルの複数の吐出孔から溶剤を含む水溶液で満たされた凝固浴に吐出して凝固繊維束とし、前記凝固繊維束は繊維としての強力を付与し、かつ脱溶剤をさせるため少なくとも1槽の洗浄槽で洗浄すると共に延伸する。該洗浄槽の溶剤は原液に含まれる溶剤と同一溶剤の水溶液であることが、溶剤回収などから有利であり、洗浄槽が多段の場合は、後段の洗浄槽になる程、溶剤濃度が低下する。温度は後段の洗浄槽になる程、高温度にすることが脱溶剤、延伸の両方を満足させるのに一般的である。
一方、近年生産性向上の要求が急速に高まり、総繊度の太繊度化、高速化による生産性向上が図られてきた。しかしながら、総繊度の太繊度化、あるいは高速化すれば洗浄槽中での洗浄液の浸透が不十分になり脱溶剤が不足するという懸念が生じる。同時に、溶液の浸透が不十分になることで凝固糸束温度が中心まで上昇しないため延伸斑あるいは、糸切れを生じ、工程トラブルを引き起こすばかりか、分繊性が悪化しローラー等への膠着糸まで生ずることがある。
In general, in the production process of acrylic fibers, a polymer solution in which a polymer is dissolved in a solvent is discharged from a plurality of discharge holes of a spinning nozzle to a coagulation bath filled with an aqueous solution containing a solvent to obtain a coagulated fiber bundle. In order to impart strength as a fiber and to remove the solvent, it is washed in at least one washing tank and stretched. It is advantageous from the viewpoint of solvent recovery that the solvent in the washing tank is an aqueous solution of the same solvent as the solvent contained in the stock solution. When there are multiple washing tanks, the concentration of the solvent decreases as the subsequent washing tank is used. . It is common that the temperature becomes higher as the washing tank in the latter stage is satisfied in order to satisfy both the solvent removal and the stretching.
On the other hand, in recent years, demands for improving productivity have increased rapidly, and productivity has been improved by increasing the total fineness and increasing the speed. However, if the total fineness is increased or the speed is increased, there is a concern that the penetration of the cleaning liquid in the cleaning tank becomes insufficient and the solvent removal becomes insufficient. At the same time, due to insufficient penetration of the solution, the temperature of the coagulated yarn bundle does not rise to the center. May occur.
特許文献１には、上記問題点に対して工程中の浴槽に於いて少なくとも一つの浴槽の槽入ローラー前と槽出ローラー後の凝固繊維束を該浴槽の一つ後の浴槽の浴液を繊維束にシャワーする事で解決する技術が開示されている。 In Patent Document 1, the solidified fiber bundle before the tank entrance roller and after the tank exit roller of the at least one bathtub in the bathtub in the process with respect to the above problem, the bath solution of the bathtub immediately after the bathtub is used. A technique to solve by showering on a fiber bundle is disclosed.
確かに特許文献１で開示されている技術を用いることで浴槽に入る前の凝固繊維束の脱溶剤は促進されるが、例えば凝固繊維束の総繊度が大きい場合、凝固繊維束の中まで洗浄液が浸透し難いので、溶剤濃度を所望の濃度まで下げるためには、多量の洗浄液を凝固繊維束にシャワーする必要がある。その結果として、洗浄槽内の洗浄抜液量が増大し、洗浄槽内で本来発揮されるべき脱溶剤効果が認められなくなるという問題が生じる。 Certainly, by using the technique disclosed in Patent Document 1, the solvent removal of the coagulated fiber bundle before entering the bathtub is promoted. For example, when the total fineness of the coagulated fiber bundle is large, the cleaning liquid is brought into the coagulated fiber bundle. Therefore, in order to reduce the solvent concentration to a desired concentration, it is necessary to shower a large amount of cleaning liquid on the coagulated fiber bundle. As a result, there arises a problem that the amount of washing drained in the washing tank increases, and the solvent removal effect that should be originally exhibited in the washing tank is not recognized.
一般的には凝固繊維は延伸されるに従って凝固浴で付着した溶剤が繊維間内部に浸透するため、後の工程になるにつれて脱溶剤し難くなる。それゆえ、前洗浄部の付与場所は重要な課題になってくるが特許文献１では、第３紡糸浴の前後で洗浄液を付与しているが、第４紡糸浴までに６倍延伸しており、数倍延伸された凝固繊維束に洗浄液を付与している。特許文献１の第１図を見る限りではシャワー液の付与場所は洗浄槽の直近であり、２つ先の紡糸浴の浴液を抜き出していることから、工程全体としての脱溶剤効率を低減させている。 In general, as the coagulated fiber is drawn, the solvent adhered in the coagulation bath penetrates into the interior of the fiber, so that it becomes difficult to remove the solvent in the subsequent process. Therefore, the location of the pre-cleaning section is an important issue, but in Patent Document 1, the cleaning liquid is applied before and after the third spinning bath, but it is stretched 6 times before the fourth spinning bath. The cleaning liquid is applied to the coagulated fiber bundle that has been stretched several times. As far as seeing FIG. 1 of Patent Document 1, the place where the shower liquid is applied is in the immediate vicinity of the washing tank, and the bath liquid of the second spinning bath is drawn out, so that the solvent removal efficiency of the entire process is reduced. ing.
前記課題は本発明によって解決される。
本発明は、アクリル系重合体が溶剤に溶解したアクリル系重合体溶液を紡糸ノズルの吐出孔から凝固浴中に吐出し、凝固浴中で凝固した凝固繊維束を凝固浴から引き上げ、洗浄槽に貯留された洗浄液中に導入して溶剤を除去する工程を有するアクリル繊維束の製造方法であって、
前記凝固繊維束が凝固浴から引き上げられた凝固繊維束に、前記洗浄槽から送液された洗浄液を付与する前洗浄工程を有し、
洗浄液が付与される凝固繊維束の速度が、凝固浴から引き上げられる凝固繊維束の引き上げ速度に対して０．８倍〜１．２倍であるアクリル繊維束の製造方法である。
The above problems are solved by the present invention.
In the present invention, an acrylic polymer solution in which an acrylic polymer is dissolved in a solvent is discharged from a discharge hole of a spinning nozzle into a coagulation bath, and a coagulated fiber bundle coagulated in the coagulation bath is pulled up from the coagulation bath and is put into a washing tank. A method for producing an acrylic fiber bundle having a step of removing the solvent by introducing it into the stored cleaning liquid,
A pre-cleaning step of applying a cleaning liquid fed from the cleaning tank to the coagulated fiber bundle in which the coagulated fiber bundle is pulled up from the coagulation bath;
This is a method for producing an acrylic fiber bundle in which the speed of the coagulated fiber bundle to which the cleaning liquid is applied is 0.8 to 1.2 times the pulling speed of the coagulated fiber bundle pulled from the coagulation bath.
本発明のアクリル繊維束の製造方法は、前記前洗浄工程にて凝固繊維束に付与する洗浄液の温度が４０℃以上９８℃以下であることが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, the temperature of the cleaning liquid applied to the coagulated fiber bundle in the pre-cleaning step is preferably 40 ° C. or higher and 98 ° C. or lower.
本発明のアクリル繊維束の製造方法は、前記前洗浄工程において、前記洗浄液を凝固繊維束に付与する方法が、洗浄液吐出ノズルから凝固繊維束に向かって前記洗浄液を吐出して、前記凝固繊維束に前記洗浄液を付与し、その吐出線速度が２ｍ／秒以上２０ｍ／秒以下であり、前記洗浄液を凝固繊維束に付与する際の凝固繊維束の移送速度が３ｍ／分〜１５ｍ／分であることが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, in the pre-cleaning step, the method of applying the cleaning liquid to the coagulated fiber bundle discharges the cleaning liquid from the cleaning liquid discharge nozzle toward the coagulated fiber bundle, and the coagulated fiber bundle And the discharge linear velocity is 2 m / second or more and 20 m / second or less, and the transfer speed of the coagulated fiber bundle when applying the cleaning liquid to the coagulated fiber bundle is 3 m / min to 15 m / min. It is preferable.
本発明のアクリル繊維束の製造方法は、前記前洗浄工程において、凝固繊維束に洗浄液を付与する位置が凝固繊維束の進行方向に２箇所以上あることが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, in the pre-cleaning step, it is preferable that there are two or more positions where the cleaning liquid is applied to the coagulated fiber bundle in the traveling direction of the coagulated fiber bundle.
本発明のアクリル繊維束の製造方法は、２箇所以上ある洗浄液を付与する前記位置間の各距離が２００ｍｍ以上であることが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, it is preferable that each distance between the positions where the cleaning liquid is applied at two or more locations is 200 mm or more.
本発明のアクリル繊維束の製造方法は、前洗浄工程において、水平に走行している凝固繊維束に対して洗浄液を付与することが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, it is preferable to apply a cleaning liquid to the coagulated fiber bundle running horizontally in the pre-cleaning step.
本発明のアクリル繊維束の製造方法は、前洗浄工程において前記洗浄液を凝固繊維束に付与する位置から１ｍ以上後に、前記凝固繊維束を前記洗浄槽に導入することが好ましい。 In the method for producing an acrylic fiber bundle of the present invention, it is preferable that the coagulated fiber bundle is introduced into the cleaning tank after 1 m or more from the position where the cleaning liquid is applied to the coagulated fiber bundle in the pre-cleaning step.
本発明のアクリル繊維束の製造方法は、凝固繊維束の繊維本数が１０００本以上８００００本以下であることが好ましい。 In the method for producing an acrylic fiber bundle according to the present invention, the number of fibers of the coagulated fiber bundle is preferably 1000 or more and 80000 or less.
本発明によれば、効率良く凝固繊維束中の溶剤を脱溶剤できる。工程全体として脱溶剤が促進されることから、洗浄槽のみで脱溶剤する場合と比較して洗浄に使用するトータルの洗浄液の量を減らすことができる。 According to the present invention, the solvent in the coagulated fiber bundle can be efficiently removed. Since solvent removal is promoted as a whole process, the total amount of cleaning liquid used for cleaning can be reduced as compared with the case where solvent removal is performed only in the cleaning tank.
以下、本発明の実施の形態について、図面を参照しながら詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
図１はこの発明の製造工程の概略図である。凝固浴１および第一洗浄槽６にはそれぞれ濃度が異なるが共に同一の溶剤の水溶液が入っている。アクリル系重合体溶液は紡糸ノズル２の吐出孔から凝固浴１に吐出され、凝固液中で凝固した凝固繊維束は第1のローラー４により引き上げられる。第1のローラーを通過した凝固繊維束は、前洗浄部８にて洗浄槽６に入る前に洗浄液が付与される。その際に使用される洗浄液は後段の洗浄槽６より配管７を通って汲み上げられる。前洗浄部を通過した凝固繊維束は、第２のローラー５、第３のローラー９を通過し、第一洗浄槽６内に導入され、さらに脱溶剤が促進される。 FIG. 1 is a schematic view of the manufacturing process of the present invention. The coagulation bath 1 and the first cleaning tank 6 contain aqueous solutions of the same solvent, both having different concentrations. The acrylic polymer solution is discharged from the discharge hole of the spinning nozzle 2 to the coagulation bath 1, and the coagulated fiber bundle coagulated in the coagulation liquid is pulled up by the first roller 4. The coagulated fiber bundle that has passed through the first roller is given a cleaning liquid before entering the cleaning tank 6 in the pre-cleaning section 8. The cleaning liquid used at that time is pumped up from the subsequent cleaning tank 6 through the pipe 7. The coagulated fiber bundle that has passed through the pre-cleaning section passes through the second roller 5 and the third roller 9 and is introduced into the first cleaning tank 6 to further promote solvent removal.
通常その後に図示されていない洗浄槽が複数あり、延伸ローラー１０を通過した後に乾燥処理が施され、ボビンに巻き取られる、またはケンスに収納される。 Usually, there are a plurality of cleaning tanks not shown in the figure, and after passing through the stretching roller 10, a drying process is performed, and the film is wound around a bobbin or stored in a can.
（凝固浴）
ここで凝固浴とは溶剤と水とからなる水溶液である。溶剤としては、ジメチルアセトアミド（以下、ＤＭＡｃと略す）、ジメチルホルムアミド、ジメチルスルホキシドなどが使用でき、アクリロニトリル重合体を溶解できるものであれば、限定されない。溶解性の観点から、ジメチルアセトアミドが好ましい。
溶剤濃度は、６０〜７０質量％が好ましい。また凝固浴の温度は３０〜４０℃が好ましい。そのような溶剤濃度及び凝固浴温度であれば、ボイドが少なく緻密な構造を形成できるからである。凝固浴では原料ポリマーを溶かしていた溶剤が凝固浴に拡散し、ポリマーが凝固し、繊維状に形成される。
(Coagulation bath)
Here, the coagulation bath is an aqueous solution comprising a solvent and water. As the solvent, dimethylacetamide (hereinafter abbreviated as DMAc), dimethylformamide, dimethylsulfoxide and the like can be used, and any solvent can be used as long as it can dissolve the acrylonitrile polymer. From the viewpoint of solubility, dimethylacetamide is preferred.
The solvent concentration is preferably 60 to 70% by mass. The temperature of the coagulation bath is preferably 30 to 40 ° C. This is because such a solvent concentration and coagulation bath temperature can form a dense structure with few voids. In the coagulation bath, the solvent dissolving the raw material polymer diffuses into the coagulation bath, and the polymer coagulates to form a fiber.
（第１のローラー）
凝固浴中の凝固繊維束は、第１のローラーを通り、空気中に引き上げられる。第１のローラーは溝付きのフリーローラーが好ましく、凝固繊維束の滑りを防止するために梨地表面となっていることが好ましい。
(First roller)
The coagulated fiber bundle in the coagulation bath passes through the first roller and is pulled up into the air. The first roller is preferably a grooved free roller, and preferably has a satin surface in order to prevent the solidified fiber bundle from slipping.
（第２のローラー）
第２のローラーは駆動ロールが好ましく、本ロールが凝固浴からの引き上げ速度を決定している。
(Second roller)
The second roller is preferably a drive roll, and this roll determines the pulling rate from the coagulation bath.
（第３のローラー）
凝固繊維束のたるみを防止するため、第２のローラー以降で凝固繊維束の温度を上げずにそのままの環境雰囲気下でわずかに延伸するのが一般的である。
(Third roller)
In order to prevent the slack of the coagulated fiber bundle, it is general that the coagulated fiber bundle is slightly stretched in the ambient atmosphere without increasing the temperature of the coagulated fiber bundle after the second roller.
(その後の洗浄槽)
通常、脱溶剤を促進させるために複数の洗浄槽があり、後段になる程洗浄槽中の水溶液の溶剤濃度が低下する一方で高温度にする。
(Subsequent washing tank)
Usually, there are a plurality of washing tanks for promoting the solvent removal, and the solvent concentration of the aqueous solution in the washing tank is lowered and the temperature is increased as it becomes later.
（延伸工程）
凝固繊維束は複数の洗浄槽を通過すると同時に洗浄槽出口の延伸ローラーで引き取られながら延伸される。
(Stretching process)
The coagulated fiber bundle passes through the plurality of washing tanks and is drawn while being drawn by a drawing roller at the washing tank outlet.
（乾燥工程）
洗浄槽を通過した後の凝固繊維束は乾燥ロールと呼ばれる蒸気を熱媒体とした加熱ロール上を通過して乾燥される。
(Drying process)
The bundle of coagulated fibers after passing through the washing tank is dried by passing on a heating roll using steam as a heat medium called a drying roll.
(前洗浄工程)
前述した通り、図２に示すＢ部では既に凝固繊維束は延伸されており溶剤の繊維間内部への浸透が進行している状態であるため、延伸がかかっていないＡ部で前洗浄することで脱溶剤が促進される。
(Pre-cleaning process)
As described above, since the coagulated fiber bundle has already been stretched in the part B shown in FIG. 2 and the penetration of the solvent into the interior of the fiber is progressing, pre-washing in the part A where no stretching is applied. The solvent removal is promoted.
前洗浄工程では、引き上げ速度に対して０．８〜１．２倍の速度で移送される凝固繊維束に第一洗浄槽から送液された洗浄液を付与する。
引き上げ速度は、第１のローラーの表面速度とする。
前洗浄工程で洗浄液を付与する凝固繊維束の速度が、引上げ速度に対して０．８〜１．２倍であれば、延伸がかかっていないか、張力の低い状態の凝固繊維束に洗浄液を付与することになり、繊維間の内部まで洗浄液が浸透しやすく、繊維間内部の溶剤と置換しやすくなる。また凝固浴あがりの凝固繊維束は繊維束表面に溶剤を大量に保持しているため、脱溶剤し易い状態となっている。
一般的には凝固繊維束は延伸されるに従って凝固浴で付着した溶剤が繊維間内部に浸透するため、後の工程になるにつれて脱溶剤し難くなる。前記速度は、引上げ速度に対して０．９〜１．１倍がより好ましく、０．９５〜１．０５倍がさらに好ましい。
In the pre-cleaning step, the cleaning liquid fed from the first cleaning tank is applied to the coagulated fiber bundle transported at a speed of 0.8 to 1.2 times the pulling speed.
The pulling speed is the surface speed of the first roller.
If the speed of the coagulated fiber bundle to which the cleaning liquid is applied in the pre-cleaning step is 0.8 to 1.2 times the pulling speed, the cleaning liquid is applied to the coagulated fiber bundle that is not stretched or has a low tension. Therefore, the cleaning liquid easily penetrates into the space between the fibers, and easily replaces the solvent inside the fibers. Further, the coagulated fiber bundle after the coagulation bath is in a state where it is easy to remove the solvent because a large amount of solvent is held on the surface of the fiber bundle.
Generally, as the coagulated fiber bundle is stretched, the solvent adhering in the coagulation bath penetrates into the interior of the interfibers, so that it becomes difficult to remove the solvent as it becomes a later step. The speed is more preferably 0.9 to 1.1 times, more preferably 0.95 to 1.05 times the pulling speed.
前洗浄工程に用いる洗浄液は、洗浄槽が複数ある場合、一番上流側の洗浄槽の洗浄液を付与するのが、洗浄液全体の量を減らせるので好ましい。 When there are a plurality of cleaning tanks, the cleaning liquid used in the pre-cleaning step is preferably applied with the cleaning liquid in the most upstream cleaning tank because the amount of the entire cleaning liquid can be reduced.
前洗浄部８にて凝固繊維束に付与する洗浄液の温度は４０℃以上９８℃以下が好ましい。４０℃以上であれば常温と比較して脱溶剤量が増加するという点で好ましく、さらに好ましくは６０℃以上である。上限としては、洗浄液が沸騰して揮発することを抑制するために９８℃以下が好ましく８０℃以下がより好ましい。 The temperature of the cleaning liquid applied to the coagulated fiber bundle in the pre-cleaning section 8 is preferably 40 ° C or higher and 98 ° C or lower. If it is 40 degreeC or more, it is preferable at the point that the amount of solvent removal increases compared with normal temperature, More preferably, it is 60 degreeC or more. As an upper limit, in order to suppress that a washing | cleaning liquid boils and volatilizes, 98 degrees C or less is preferable and 80 degrees C or less is more preferable.
前洗浄部８にて付与する洗浄液の吐出線速度は２ｍ/秒以上２０ｍ/秒以下であることが好ましい。前記吐出線速度が２ｍ/秒以上であれば凝固繊維束の内部まで洗浄液が浸透するという点で好ましく、２０ｍ/秒以下であれば単繊維が切断し毛羽になることを防ぎやすくなる。前記吐出線速度は５ｍ/秒以上１６ｍ/秒以下がより好ましく、８ｍ/秒以上１２ｍ/秒以下がさらに好ましい。ここで、吐出線速度とは配管７の先端に吐出ノズルあるいはナイロンチューブを装着し、その吐出ノズルあるいはナイロンチューブ開口部から放出された直後の洗浄液の速度を言う。吐出線速度は、前記開口部から単位時間当たりに吐出される洗浄液の量を、前記開口部の面積で除することで算出する。 The discharge linear velocity of the cleaning liquid applied by the pre-cleaning unit 8 is preferably 2 m / second or more and 20 m / second or less. If the discharge linear velocity is 2 m / sec or more, it is preferable in that the cleaning liquid penetrates into the solidified fiber bundle, and if it is 20 m / sec or less, it becomes easy to prevent the single fibers from being cut and becoming fluff. The discharge linear velocity is more preferably 5 m / sec or more and 16 m / sec or less, and further preferably 8 m / sec or more and 12 m / sec or less. Here, the discharge linear velocity means the velocity of the cleaning liquid immediately after the discharge nozzle or nylon tube is attached to the tip of the pipe 7 and discharged from the discharge nozzle or nylon tube opening. The discharge linear velocity is calculated by dividing the amount of cleaning liquid discharged from the opening per unit time by the area of the opening.
[計算例]
後述の実施例１で吐出線速度を９．４m/sと算出した、実際の計算例を示す。実施例１にて設定した洗浄液の付与量は１．０Ｌ／分であり、使用したノズルはスプレーイングシステム社製の型番：Ｂ１／８ＨＨ−ｓｓ＾３である。該ノズルのオリフィス呼び径は１．５ｍｍであることから、開口面積は１．７７×１０−２ｃｍ２となる。従って、吐出線速度は１０００ｃｍ３／分÷（１．７７×１０−２）ｃｍ２＝５．６５×１０４ｃｍ／分＝９．４ｍ／秒となる。
[Calculation example]
An actual calculation example in which the discharge linear velocity is calculated as 9.4 m / s in Example 1 described later will be shown. The application amount of the cleaning liquid set in Example 1 is 1.0 L / min, and the nozzle used is Model No. B1 / 8HH-ss ^ 3 manufactured by Spraying System. Since the nominal orifice diameter of the nozzle is 1.5 mm, the opening area is 1.77 × 10 −2 cm 2 . Therefore, the discharge linear velocity is 1000 cm 3 /min÷(1.77×10 −2 ) cm 2 = 5.65 × 10 4 cm / min = 9.4 m / sec.
前洗浄部８にて凝固繊維束に洗浄液を付与する場所は、凝固繊維束の進行方向に対して２００ｍｍ以上離して２箇所に分割して付与することが好ましい。ここで離すとは２箇所それぞれに配置した吐出ノズル間を結んだ工程に配置された凝固繊維束の長さが２００ｍｍ以上の長さになることを言う。そうすることで、１段目で付与した液は内部からの溶剤の拡散を促し、２箇所目でさらに洗浄されることでより高い脱溶剤効果が発揮されるためである。吐出ノズルの配置について、１箇所目は引き上げ速度に対して０．８〜１．２倍の速度で移送される間に配置するが、２段目の配置箇所については制限を設けないが、２段目も０．８〜１．２倍の速度で移送される間に配置するのが好ましい。 The place where the cleaning liquid is applied to the coagulated fiber bundle in the pre-cleaning section 8 is preferably divided and applied in two places separated by 200 mm or more with respect to the traveling direction of the coagulated fiber bundle. Here, separating means that the length of the coagulated fiber bundle arranged in the process of connecting the discharge nozzles arranged at two places becomes 200 mm or more. By doing so, it is because the liquid given at the first stage promotes the diffusion of the solvent from the inside, and is further washed at the second place, so that a higher solvent removal effect is exhibited. Regarding the arrangement of the discharge nozzles, the first part is arranged while being transferred at a speed of 0.8 to 1.2 times the pulling speed, but there is no restriction on the arrangement part of the second stage. It is preferable to arrange the stage while it is transported at a speed of 0.8 to 1.2 times.
前洗浄工程において水平に走行している凝固繊維束に対して洗浄液を付与することが好ましい。水平に走行している凝固繊維束に対して洗浄液を付与すると、洗浄液が繊維間に浸透し易くなる。 It is preferable to apply a cleaning liquid to the coagulated fiber bundle running horizontally in the pre-cleaning step. When the cleaning liquid is applied to the coagulated fiber bundle running horizontally, the cleaning liquid easily penetrates between the fibers.
前洗浄工程における凝固繊維束に洗浄液を付与する位置は、洗浄槽に凝固繊維束が導入される１ｍ以上手前の位置であることが好ましい。 前記の１ｍ以上手前の位置とは、前洗浄工程における凝固繊維束に洗浄液を付与する位置から、洗浄槽の洗浄液中に凝固繊維束が導入される位置までを凝固繊維束が移送する距離が１ｍ以上となる位置を言う。前記位置で凝固繊維束に洗浄液を付与すると洗浄液が凝固繊維束の繊維間に浸透し洗浄効果が高くなり易いためである。 The position where the cleaning liquid is applied to the coagulated fiber bundle in the pre-cleaning step is preferably a position 1 m or more before the coagulated fiber bundle is introduced into the cleaning tank. The position 1 m or more in front is a distance of 1 m from which the coagulated fiber bundle is transferred from the position where the cleaning liquid is applied to the coagulated fiber bundle in the pre-cleaning process to the position where the coagulated fiber bundle is introduced into the cleaning liquid in the cleaning tank. The position which becomes the above is said. This is because when the cleaning liquid is applied to the coagulated fiber bundle at the above position, the cleaning liquid penetrates between the fibers of the coagulated fiber bundle and the cleaning effect is likely to be enhanced.
本発明に用いる凝固繊維束の繊維本数は、１０００本以上８００００本以下が好ましい。１０００本以上であれば、本発明の前洗浄によるトータルの洗浄液削減効果が得られやすい。また、８００００本以下であれば、前洗浄による脱溶剤が促進されやすいので好ましい。繊維本数は、前記観点から１００００本〜６００００本がより好ましく、１３０００本〜３００００本がさらに好ましい。 The number of fibers of the coagulated fiber bundle used in the present invention is preferably 1000 or more and 80000 or less. If it is 1000 or more, it is easy to obtain the total cleaning liquid reduction effect by the pre-cleaning of the present invention. Moreover, if it is 80000 or less, since the solvent removal by pre-cleaning is easy to be accelerated | stimulated, it is preferable. The number of fibers is more preferably 10,000 to 60000 from the above viewpoint, and further preferably 13000 to 30000.
＜脱溶剤率の測定方法＞
前洗浄工程における凝固繊維束からの脱溶剤率は以下の手順で測定する。
・ バットを前洗浄工程部の洗浄液落下部に設置する。
・ 前洗浄工程部では付与した洗浄液は凝固繊維束を洗浄した後に落下するため、その落下液を1分間バットで受ける。
・ 得られた液の濃度ｃ[％]と落下液流量Ｌ[ｇ／分]を測定する。得られた液の濃度の測定の際には屈折率計を使用し、落下液量の測定の際には電子天秤で秤量することにより求めた。
・ 第一洗浄槽の濃度をｃ１[％%]とすると前洗浄工程で脱落した溶剤量はＬ×（ｃ−ｃ１）／１００[ｇ／分]となる。
<Measurement method of solvent removal rate>
The solvent removal rate from the coagulated fiber bundle in the pre-cleaning step is measured by the following procedure.
・ Install the vat in the cleaning liquid dropping section of the pre-cleaning process section.
-In the pre-cleaning process section, the applied cleaning solution falls after cleaning the coagulated fiber bundle, so that the falling solution is received with a vat for 1 minute.
-Measure the concentration c [%] and the falling liquid flow rate L [g / min] of the obtained liquid. A refractometer was used when measuring the concentration of the obtained liquid, and it was determined by weighing with an electronic balance when measuring the amount of falling liquid.
Solvent amount the concentration of the first cleaning tank dropped in the pre-cleaning process when the c 1 [%%] becomes L × (c-c 1) / 100 [g / min].
（実施例１）
以下、本発明の実施例について説明する。アクリロニトリル９６．５質量％、アクリルアミド２．７質量％、メタクリル酸０．８質量％からなるアクリル系重合体を、アクリル系重合体２１．２質量％、ジメチルアセトアミド７８．８質量％の比率で混合溶解しアクリル系重合体溶液を得た。前記アクリル系重合体溶液を吐出孔径が０．０７５ｍｍφである吐出孔を１５０００個有する紡糸ノズルの吐出孔から吐出量が１８０ｇ／分で、ＤＭＡｃ／水＝６７／３３質量％、３８℃の凝固浴中に吐出して凝固繊維束とし、前記凝固繊維束を第１ロールを通って、駆動ロールである第２のローラーで引き上げた。引き上げ速度となる第１ローラーの表面速度は、８．０ｍ／分であった。第１ローラー４と第２ローラー５との間の凝固繊維束の移送速度は引き上げ速度に対して１．０倍の速度である。第１ローラー４と第２のローラー５との間（図２中のＡ部）の凝固繊維束に、前洗浄工程として第一洗浄槽の底部より抜き出した洗浄液を付与した。洗浄液温度は６５℃、洗浄液のＤＭＡｃ濃度は１８．７質量％、吐出ノズルからの洗浄液の吐出量は１．０Ｌ／分、ノズルから噴出す洗浄液の圧力は５０ＫＰａ、吐出線速度は９．４ｍ／秒であった。使用したノズルはスプレーイングシステム社製の型番：Ｂ１／８ＨＨ−ｓｓ−３である。その後第２のローラー５と第３のローラー９の間で１．３倍に延伸し、６５℃、ＤＭＡｃ濃度１８．７％の第一洗浄槽６に導入した。
前洗浄工程での脱溶剤率を表１に示す。
Example 1
Examples of the present invention will be described below. An acrylic polymer composed of 96.5% by mass of acrylonitrile, 2.7% by mass of acrylamide, and 0.8% by mass of methacrylic acid was mixed in a ratio of 21.2% by mass of the acrylic polymer and 78.8% by mass of dimethylacetamide. Dissolved to obtain an acrylic polymer solution. A coagulation bath of the acrylic polymer solution having a discharge rate of 180 g / min, DMAc / water = 67/33 mass%, 38 ° C. from the discharge holes of a spinning nozzle having 15,000 discharge holes having a discharge hole diameter of 0.075 mmφ. The solidified fiber bundle was discharged into the solidified fiber bundle, and the solidified fiber bundle passed through the first roll and was pulled up by the second roller as the drive roll. The surface speed of the first roller serving as the pulling speed was 8.0 m / min. The transfer speed of the solidified fiber bundle between the first roller 4 and the second roller 5 is 1.0 times the pulling speed. The cleaning liquid extracted from the bottom of the first cleaning tank was applied to the coagulated fiber bundle between the first roller 4 and the second roller 5 (A part in FIG. 2) as a pre-cleaning step. The cleaning liquid temperature is 65 ° C., the DMAc concentration of the cleaning liquid is 18.7% by mass, the discharge amount of the cleaning liquid from the discharge nozzle is 1.0 L / min, the pressure of the cleaning liquid ejected from the nozzle is 50 KPa, and the discharge linear velocity is 9.4 m / Second. The used nozzle is model number: B1 / 8HH-ss-3 manufactured by Spraying System. Thereafter, the film was stretched 1.3 times between the second roller 5 and the third roller 9 and introduced into the first cleaning tank 6 at 65 ° C. and DMAc concentration of 18.7%.
Table 1 shows the solvent removal rate in the pre-cleaning step.
[計算例]
脱溶剤率を２７．２％と算出した実際の計算例を示す。
実施例１に示すように、アクリル系重合体溶液は紡糸ノズルの吐出孔から吐出量が１８０ｇ／分でＤＭＡｃ６７％の濃度の凝固浴に吐出される。凝固浴から引き上げられた凝固繊維束の含水分率［＝（凝固浴あがり凝固繊維束（ｇ）／絶乾凝固繊維束（ｇ））×１００］は２５０質量％であり、凝固繊維束に付着している溶剤濃度は凝固浴と同一、すなわち６７％のＤＭＡｃであることから凝固繊維束が保有しているＤＭＡｃ総量は１８０×６７／１００×２５０／１００＝３０１．５ｇ／分である。
一方、前洗浄工程で脱落した溶剤量を求めるために凝固繊維束を洗浄した後に落下する液の流量とその濃度を測定すると、それぞれ７６２．８ｇ／分、２９．４７%であった。従って、前洗浄工程で脱落した溶剤量は７６２．８×(２９．４７−１８．７)／１００＝８２．１ｇ／分である。
脱溶剤率を（脱落した溶剤量）÷（前洗浄する前の凝固繊維束の保有溶剤量）×１００と定義すると、本実施例での前洗浄工程での脱溶剤率は８２．１÷３０１．５×１００＝２７．２％となる。なお、前洗浄工程で凝固繊維束の保有溶剤が全て脱落した場合には脱溶剤率は１００％となる。一般的に複数段の洗浄槽を通過した後は脱溶剤率がほぼ１００％になるよう生産条件を決定している。
[Calculation example]
An actual calculation example in which the solvent removal rate is calculated as 27.2% is shown.
As shown in Example 1, the acrylic polymer solution is discharged from the discharge hole of the spinning nozzle into a coagulation bath having a concentration of DMAc of 67% at a discharge rate of 180 g / min. The moisture content of the coagulated fiber bundle pulled up from the coagulation bath [= (coagulation bath up coagulated fiber bundle (g) / absolutely coagulated fiber bundle (g)) × 100] is 250% by mass and adheres to the coagulated fiber bundle. Since the solvent concentration is the same as that of the coagulation bath, that is, 67% DMAc, the total amount of DMAc held by the coagulated fiber bundle is 180 × 67/100 × 250/100 = 301.5 g / min.
On the other hand, when the flow rate and the concentration of the liquid dropped after washing the coagulated fiber bundle were measured in order to determine the amount of the solvent dropped off in the pre-cleaning step, they were 762.8 g / min and 29.47%, respectively. Therefore, the amount of the solvent dropped out in the pre-cleaning step is 762.8 × (29.47-18.7) /100=82.1 g / min.
When the solvent removal rate is defined as (amount of solvent dropped off) / (amount of solvent in the coagulated fiber bundle before pre-cleaning) × 100, the solvent removal rate in the pre-cleaning step in this example is 82.1 ÷ 301. .5 × 100 = 27.2%. In addition, when all the solvent possessed by the coagulated fiber bundle is removed in the pre-cleaning step, the solvent removal rate is 100%. Generally, after passing through a plurality of stages of washing tanks, the production conditions are determined so that the solvent removal rate is almost 100%.
（実施例２）
前洗浄工程の洗浄液付与位置を２段にし、前記位置を３００ｍｍ離間し、それぞれのノズルから噴出す洗浄液の圧力を１００ＫＰａ、洗浄液の付与量を０．５Ｌ／分、使用ノズルをスプレーイングシステム社製のＢ１／８ＨＨ−ｓｓ−１とした以外は、実施例1と同様の作製方法でアクリル繊維束を製造した。この時、２段目の付与場所も引き上げ速度に対して１．０倍で凝固繊維束が移送されているＡ部である。
その結果を表１に示す。この結果より２段付与の場合も十分な脱溶剤効果が発揮されることが分かる。
(Example 2)
The cleaning liquid application position in the pre-cleaning process is set in two stages, the positions are separated by 300 mm, the pressure of the cleaning liquid ejected from each nozzle is 100 KPa, the application amount of the cleaning liquid is 0.5 L / min, and the nozzle used is made by Spraying System An acrylic fiber bundle was produced by the same production method as in Example 1 except that B1 / 8HH-ss-1 was used. At this time, the application position of the second stage is also the A part where the coagulated fiber bundle is transferred at 1.0 times the pulling speed.
The results are shown in Table 1. From this result, it is understood that a sufficient solvent removal effect is exhibited even in the case of two stages.
（実施例３）
実施例１と同様の作製方法で得られたアクリル系重合体溶液を吐出孔数６０００ホール、吐出孔径０．０７５ｍｍφの口金を用いて、吐出量４６９．０ｇ／分、引き上げ速度４．０ｍ／分の条件とし、前洗浄工程として図２中のＡ部に第一洗浄槽の洗浄液を底部より抜き出し、スプレーノズルを使用して吐出線速度６．８ｍ／秒、６５℃、５０ＫＰａ、０．２Ｌ／分で付与した以外は、実施例１と同様の作製方法でアクリル繊維束を製造した。なお、スプレーノズルはスプレーイングシステム社製の型番：Ｂ１／８Ｇ−３００１．４のノズルを使用した。
(Example 3)
The acrylic polymer solution obtained by the same production method as in Example 1 was used with a nozzle having a discharge hole number of 6000 holes and a discharge hole diameter of 0.075 mmφ, a discharge amount of 469.0 g / min, and a lifting speed of 4.0 m / min. As a pre-cleaning step, the cleaning liquid in the first cleaning tank is extracted from the bottom at part A in FIG. 2, and a spray nozzle is used to discharge a linear velocity of 6.8 m / second, 65 ° C., 50 KPa, 0.2 L / An acrylic fiber bundle was produced by the same production method as in Example 1 except that it was applied in minutes. In addition, the spray nozzle used the nozzle of the spraying system company type | model number: B1 / 8G-3001.4.
（実施例４）
前洗浄部で配管７の先端の洗浄液の付与方法をスプレーノズルではなく、内径６ｍｍのナイロンチューブを１本用いて、吐出線速度を０．１ｍ／秒として吐出した以外は実施例３と同様にして、アクリル繊維束を得た。ナイロンチューブを使用する際は吐出圧は０ＫＰａとなる。
Example 4
The method of applying the cleaning liquid at the tip of the pipe 7 in the pre-cleaning section was the same as in Example 3 except that one nylon tube with an inner diameter of 6 mm was used instead of a spray nozzle and the discharge linear velocity was 0.1 m / sec. Thus, an acrylic fiber bundle was obtained. When a nylon tube is used, the discharge pressure is 0 KPa.
その結果、表１に示すように吐出線速度が６．８ｍ／秒の時には十分な脱溶剤効果が発揮されるが、吐出線速度０．１ｍ／秒の時は洗浄効果が低下するが、洗浄槽の直前で洗浄液を付与する場合に比較すると、洗浄効果は高いことが分かる。 As a result, as shown in Table 1, a sufficient solvent removal effect is exhibited when the discharge linear velocity is 6.8 m / sec, but the cleaning effect is reduced when the discharge linear velocity is 0.1 m / sec. It can be seen that the cleaning effect is high compared to the case where the cleaning liquid is applied immediately before the tank.
（実施例５）
実施例１と同様の作製方法で得られたクリル系重合体溶液を、吐出孔数１２０００ホール、吐出孔径０．０７５ｍｍφの口金を用いて、吐出量２９０ｇ／分、引き上げ速度４．０ｍ／分の条件下で、ＤＭＡｃ／水＝６７／３３質量％、３８℃の凝固浴に紡出した。凝固浴から引き上げられた凝固繊維束は図1中の第２のローラー５を通過して、６５℃、ＤＭＡｃ濃度０％の第一洗浄槽６にて脱溶剤する。なお、本実施例では温度による効果を確認するために意図的に第一洗浄槽中の溶媒を純水に置換している。前洗浄工程として図２中のＡ部に第一洗浄槽の洗浄液を底部より抜き出し、０．３Ｌ／分、５０ＫＰａ、６５℃、１０．２ｍ／秒で付与した。この間、凝固繊維束は引き取り速度に対して１．０倍の速度で移送される。前洗浄に使用したノズルはスプレーイングシステム社製の型番：Ｂ１／８ＨＨ−ｓｓ−１である。
(Example 5)
Using a nozzle having a discharge hole number of 12,000 and a discharge hole diameter of 0.075 mmφ, a kryl polymer solution obtained by the same production method as in Example 1 was discharged at a rate of 290 g / min and a lifting speed of 4.0 m / min. Under the conditions, spinning was performed in a coagulation bath of DMAc / water = 67/33 mass% and 38 ° C. The coagulated fiber bundle pulled up from the coagulation bath passes through the second roller 5 in FIG. 1 and is desolvated in the first washing tank 6 at 65 ° C. and DMAc concentration 0%. In the present embodiment, the solvent in the first cleaning tank is intentionally replaced with pure water in order to confirm the effect of temperature. As a pre-cleaning step, the cleaning liquid in the first cleaning tank was extracted from the bottom to part A in FIG. 2 and applied at 0.3 L / min, 50 KPa, 65 ° C., and 10.2 m / sec. During this time, the coagulated fiber bundle is transferred at a speed 1.0 times the take-up speed. The nozzle used for pre-cleaning is model number: B1 / 8HH-ss-1 manufactured by Spraying System.
（実施例６）
前洗浄工程として洗浄液の付与温度を２０℃とした以外は、実施例２と同様にして、アクリル繊維束を得た。
(Example 6)
An acrylic fiber bundle was obtained in the same manner as in Example 2 except that the application temperature of the cleaning liquid was 20 ° C. as the pre-cleaning step.
実施例５と実施例６との洗浄液温度の違いによる脱溶剤効果について、表１に示すように６５℃で付与する方が、脱溶剤効果が高いことが分かる。 As shown in Table 1, the solvent removal effect due to the difference in cleaning liquid temperature between Example 5 and Example 6 is higher when applied at 65 ° C.
（比較例１）
前洗浄工程として凝固繊維束に洗浄液を付与した場所を引き上げ速度に対して１．３倍となる図２中のＢ部とした以外は、実施例１と同様にして、アクリル繊維束を得た。
(Comparative Example 1)
An acrylic fiber bundle was obtained in the same manner as in Example 1 except that the place where the cleaning liquid was applied to the coagulated fiber bundle as the pre-cleaning step was set to B part in FIG. .
その結果、表１に示すように延伸がかかっているＢ部では脱溶剤効果が極端に落ちることが分かる。 As a result, as shown in Table 1, it can be seen that the solvent removal effect is extremely lowered in the portion B where the stretching is applied.
１：凝固浴
２：口金
３：凝固繊維束
４：第１のローラー
５：第２のローラー
６：第一洗浄槽
７：配管
８：前洗浄部
９：第３のローラー
10：延伸ローラー
Ａ：前洗浄工程位置
Ｂ：延伸糸への付与位置
1: coagulation bath 2: base 3: coagulated fiber bundle 4: first roller 5: second roller 6: first cleaning tank 7: pipe 8: pre-cleaning section 9: third roller
10: Stretching roller A: Pre-cleaning process position B: Position applied to the drawn yarn
Claims (8)
凝固浴から引き上げられた前記凝固繊維束に、前記洗浄槽から送液された洗浄液を付与する前洗浄工程を有し、
洗浄液が付与される凝固繊維束の速度が、凝固浴から引き上げられる凝固繊維束の引き上げ速度に対して０．８倍〜１．２倍であるアクリル繊維束の製造方法。 The acrylic polymer solution in which the acrylic polymer is dissolved in the solvent is discharged into the coagulation bath from the multiple discharge holes of the spinning nozzle, and the coagulated fiber bundle coagulated in the coagulation bath is pulled up from the coagulation bath and stored in the washing tank. A method for producing an acrylic fiber bundle having a step of removing the solvent by introducing it into the washing liquid,
A pre-cleaning step of applying a cleaning solution fed from the cleaning tank to the coagulated fiber bundle pulled up from the coagulation bath;
A method for producing an acrylic fiber bundle, wherein the speed of the coagulated fiber bundle to which the cleaning liquid is applied is 0.8 to 1.2 times the pulling speed of the coagulated fiber bundle pulled from the coagulation bath.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105908274A (en) * | 2016-05-20 | 2016-08-31 | 南通富之岛寝具发展有限公司 | Washing-force-adjustable polyester silk washing device |
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