JPH0229764B2 - - Google Patents
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- Publication number
- JPH0229764B2 JPH0229764B2 JP57041734A JP4173482A JPH0229764B2 JP H0229764 B2 JPH0229764 B2 JP H0229764B2 JP 57041734 A JP57041734 A JP 57041734A JP 4173482 A JP4173482 A JP 4173482A JP H0229764 B2 JPH0229764 B2 JP H0229764B2
- Authority
- JP
- Japan
- Prior art keywords
- spinning
- methanol
- stock solution
- weight
- concentration
- Prior art date
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Description
本発明はアセテート繊維の製造方法に関する。
更に詳しくは、セルロースジアセテートを塩化メ
チレンとメタノールとの混合物に溶解させた紡糸
原液から乾式紡糸法でアセテート繊維を製造する
方法に関する。
ジアセテート繊維は一般にアセトンまたはアセ
トンと水との混合物を溶剤とする紡糸原液から乾
式紡糸法で製造されているのに対して、トリアセ
テート繊維は塩化メチレンまたは塩化メチレンと
メタノールとの混合物を溶剤とする紡糸原液から
乾式紡糸法で製造されている。この2種のアセテ
ート繊維を製造する工場では、それぞれの溶剤の
蒸気が混ざり合わないようにして別々に回収する
ために、それぞれに独立した紡糸建屋と溶剤回収
装置とを設けている例が多い。この2種のアセテ
ート繊維を同一の紡糸建屋と溶剤回収装置とで製
造することも可能であるが、この場合には回収溶
剤の精密な蒸留を行なわなければ回収溶剤を含む
紡糸原液による紡糸工程トラブルが多発すること
となる。ジアセテート繊維を塩化メチレンまたは
塩化メチレンとメタノールとの混合物を溶剤とす
る紡糸原液から乾式紡糸法によつて製造する場合
には、ジアセテート繊維とトリアセテート繊維と
を共通の建屋と溶剤回収装置とを用いて安価に製
造することが可能となるが、この方法では紡糸工
程での断糸が多くなる欠点がある。
本発明者は、セルロースジアセテートを塩化メ
チレンとメタノールとの混合物に溶解させた紡糸
原液から乾式紡糸法でアセテート繊維を製造する
方法における紡糸工程での断糸を減少させ、これ
によつてジアセテート繊維とトリアセテート繊維
とを同一建屋内で製造することを可能ならしめる
ことを目的として鋭意検討した結果、溶剤として
使用する塩化メチレンとメタノールとの混合比率
(以下溶剤混合比率と称する。)及び紡糸原液中の
セルロースジアセテートの濃度(以下原液濃度と
称する。)の2つの因子が紡糸工程での断糸発生
率に大きな影響を及ぼし、この2つの因子がある
限定された最適範囲内にある場合には紡糸工程で
の断糸の発生が少なくなることを見いだし更に検
討して本発明に到達した。
セルロースジアセテートを塩化メチレンとメタ
ノールとの混合物からなり、この混合物中のメタ
ノールの割合が8〜15重量%である有機溶媒にセ
ルロースジアセテートの濃度が21〜24重量%にな
るように溶解して紡糸原液となし、この紡糸原液
を70〜80℃に加熱した後、VT/VE(但し、VEは
紡糸原液の紡糸ノズルからの吐出速度、VTは糸
条の引き取り速度を示す)が0.85〜0.80となる条
件下で乾式紡糸することを特徴とするアセテート
繊維の製造方法にある。
溶剤混合比率は紡糸工程での断糸発生率及び紡
糸された糸条の物性に大きな影響を及ぼす。メタ
ノールの割合が8重量%未満ではメタノールの割
合が小さくなるにつれて紡糸工程での断糸発生率
が高くなり、メタノールの割合が15%を越える領
域ではメタノールの割合が大きくなるにつれて紡
糸された糸条の強度及び伸度が低くなる。このこ
とから、メタノールの割合は8重量%以上でかつ
15重量%以下が適当である。
原液濃度もまた紡糸工程での断糸発生率及び紡
糸された糸条の物性に大きな影響を及ぼす。原液
濃度については、濃度が高いほど原液調製工程の
生産性が高くなるとともに溶剤回収に要する費用
を低減できるので、製造コストの点では原液濃度
はできるだけ高いことが望ましいが原液濃度が24
重量%を越えると紡糸工程での断糸発生率が急に
高くなるとともに紡糸された糸条の伸度が低くな
る。原液濃度が21%未満では製造コストが高くな
とともに紡糸された糸条の中に繊維断面の形状が
異常である単繊維の比率が高くなる。このことか
ら原液濃度は21重量%以上でかつ24重量%以下の
範囲が適当である。
また本発明を実施するに当つては、紡糸原液を
70℃以上でかつ80℃以下の温度に加熱した後に紡
糸ノズルから吐出させるのが好ましい。紡糸原液
の温度が高いほど紡糸された糸条の伸度が高くな
ることから紡糸工程での断糸発生率が高くならな
い範囲内で高い温度にすることが望ましい。本発
明の方法の場合には紡糸原液を80℃を越えて加熱
すると断糸の発生率がきわめて高くなりまた70℃
未満では紡糸された糸条の伸度が低くなることか
ら、70℃以上でかつ80℃以下の範囲が望ましい。
さらに本発明では、紡糸原液が紡糸ノズルから
吐出される速度VEと糸条の引き取り速度VTとの
比VT/VEが0.85を越える場合には紡速工程での
断糸発生率がきわめて高くなり、0.80未満では異
常断面発生率が高くなることからVT/VE0.85〜
0.80であることが望ましい。この速度比VT/VE
は紡糸する糸条の繊度(Dデニール)及びフイラ
メント数(F)、紡糸原液の濃度(C重量%)及
び密度(Pg/cm3)、ノズルの孔半径(rcm)と
を用いて式(1)で示されるようにr2に比例する値と
なるので、VT/VEが0.85〜0.80となるようにノズ
ル孔半径rを決めればよい。
VT/VE=A・C・P r2 F/D …(1)
(但しAは定数である。)
以下に本発明を実施例に従つてさらに詳細に説
明する。
実施例 1
第1表に示した割合で混合した塩化メチレンと
メタノールとの混合物中に所定量のセルロースジ
アセテートを溶解させた溶液を通常どおりに過
して紡糸原液となし、この紡糸原液を75℃に加熱
した後にVT/VEが0.85以下でかつ0.80以上となる
ように選んだ紡糸ノズルから吐出させ、通常の方
法で乾燥して800m/分の速度で引きとり100デニ
ール27フイラメントのアセテート繊維を得、その
結果を第1表に示した。第1表中、原液濃度は紡
糸原液中に含まれるセルロースジアセテートの割
合を重量濃度(%)で示した値であり、メタノー
ル比は塩化メチレンとメタノールとの混合物中に
含まれるメタノールの割合を重量濃度(%)で示
した値であり、断糸発生率は紡糸工程での1日
100錘当りの断糸発生回数を示した値であり、伸
度はJISで定められた方法に従つて測定した乾伸
度の値であり、異常断面発生率は繊維断面の形状
が異常であるフイラメントの割合(%)を示した
値である。尚、繊維断面が異常であるかどうかの
判定は、繊維断面を顕微鏡で観察し、凹部及び凸
部がそれぞれ3ケ以下であるフイラメントを繊維
断面が異常であるフイラメントとした。
The present invention relates to a method for producing acetate fibers.
More specifically, the present invention relates to a method for producing acetate fibers using a dry spinning method from a spinning stock solution in which cellulose diacetate is dissolved in a mixture of methylene chloride and methanol. Diacetate fibers are generally produced by dry spinning from a spinning stock solution using acetone or a mixture of acetone and water as the solvent, whereas triacetate fibers are produced using methylene chloride or a mixture of methylene chloride and methanol as the solvent. It is manufactured using the dry spinning method from spinning dope. Factories that manufacture these two types of acetate fibers often have separate spinning buildings and solvent recovery equipment in order to prevent the vapors of each solvent from mixing and recover them separately. It is also possible to produce these two types of acetate fibers in the same spinning building and solvent recovery equipment, but in this case, unless the recovered solvent is precisely distilled, problems may occur during the spinning process due to the spinning dope containing the recovered solvent. will occur frequently. When diacetate fibers are produced by a dry spinning method from a spinning stock solution using methylene chloride or a mixture of methylene chloride and methanol as a solvent, diacetate fibers and triacetate fibers are manufactured in a common building and a solvent recovery device. However, this method has the disadvantage that yarn breakage occurs frequently in the spinning process. The present inventor has devised a method for producing acetate fibers using a dry spinning method from a spinning dope in which cellulose diacetate is dissolved in a mixture of methylene chloride and methanol. As a result of intensive studies aimed at making it possible to manufacture fibers and triacetate fibers in the same building, we have determined the mixing ratio of methylene chloride and methanol used as solvents (hereinafter referred to as the solvent mixing ratio) and the spinning dope. Two factors, the concentration of cellulose diacetate in the fiber (hereinafter referred to as the concentration of the stock solution), have a large effect on the incidence of yarn breakage in the spinning process, and when these two factors are within a certain limited optimum range, found that the occurrence of yarn breakage during the spinning process was reduced, and after further investigation, they arrived at the present invention. Cellulose diacetate is dissolved in an organic solvent consisting of a mixture of methylene chloride and methanol in which the proportion of methanol in the mixture is 8 to 15% by weight so that the concentration of cellulose diacetate is 21 to 24% by weight. After heating this spinning dope to 70 to 80°C, V T /V E (where V E is the discharge speed of the spinning dope from the spinning nozzle, and V T is the take-up speed of the yarn). A method for producing acetate fiber, which comprises dry spinning under conditions such that the fiber is 0.85 to 0.80. The solvent mixing ratio has a great influence on the incidence of yarn breakage in the spinning process and the physical properties of the spun yarn. When the proportion of methanol is less than 8% by weight, as the proportion of methanol decreases, the occurrence of yarn breakage in the spinning process increases, and in the area where the proportion of methanol exceeds 15%, the proportion of spun yarn increases as the proportion of methanol increases. strength and elongation are reduced. From this, the proportion of methanol is 8% by weight or more and
A suitable content is 15% by weight or less. The concentration of the stock solution also has a large effect on the incidence of yarn breakage during the spinning process and on the physical properties of the spun yarn. Regarding the concentration of the stock solution, the higher the concentration, the higher the productivity of the stock solution preparation process and the lower the cost required for solvent recovery.From the viewpoint of manufacturing costs, it is desirable that the concentration of the stock solution is as high as possible.
If it exceeds % by weight, the incidence of yarn breakage in the spinning process will suddenly increase and the elongation of the spun yarn will decrease. If the concentration of the stock solution is less than 21%, the production cost will be high and the proportion of single fibers with abnormal fiber cross-sectional shapes in the spun yarn will be high. From this, it is appropriate that the concentration of the stock solution is in the range of 21% by weight or more and 24% by weight or less. In carrying out the present invention, the spinning stock solution is
It is preferable to discharge it from a spinning nozzle after heating it to a temperature of 70° C. or higher and 80° C. or lower. The higher the temperature of the spinning dope, the higher the elongation of the spun yarn, so it is desirable to keep the temperature high within a range that does not increase the incidence of yarn breakage in the spinning process. In the case of the method of the present invention, if the spinning dope is heated above 80°C, the incidence of yarn breakage will be extremely high;
If the temperature is less than 70°C, the elongation of the spun yarn will be low, so it is preferably in the range of 70°C or higher and 80°C or lower. Furthermore, in the present invention, if the ratio V T /V E of the speed V E at which the spinning dope is discharged from the spinning nozzle and the take-up speed V T of the yarn exceeds 0.85, the occurrence of yarn breakage in the spinning speed process is reduced. If it is less than 0.80, the incidence of abnormal cross section will be high, so V T /V E 0.85 ~
A value of 0.80 is desirable. This speed ratio V T /V E
is expressed by the formula (1) using the fineness (D denier) and number of filaments (F) of the yarn to be spun, the concentration (C weight %) and density (Pg/cm 3 ) of the spinning dope, and the nozzle hole radius (rcm). ), the nozzle hole radius r should be determined so that V T /V E is 0.85 to 0.80. V T /V E =A·C·P r 2 F/D (1) (However, A is a constant.) The present invention will be described in more detail below with reference to Examples. Example 1 A solution in which a predetermined amount of cellulose diacetate was dissolved in a mixture of methylene chloride and methanol mixed in the ratio shown in Table 1 was passed in the usual manner to obtain a spinning stock solution. After heating to ℃, it is discharged from a spinning nozzle selected so that V T /V E is 0.85 or less and 0.80 or more, dried in the usual manner, and taken off at a speed of 800 m/min to produce 100 denier 27 filament acetate. Fibers were obtained and the results are shown in Table 1. In Table 1, the stock solution concentration is the weight concentration (%) of the proportion of cellulose diacetate contained in the spinning stock solution, and the methanol ratio is the proportion of methanol contained in the mixture of methylene chloride and methanol. The value is expressed as weight concentration (%), and the yarn breakage rate is calculated based on the yarn breakage rate per day in the spinning process.
This value indicates the number of times yarn breakage occurs per 100 spindles, the elongation is the dry elongation measured according to the method specified by JIS, and the abnormal cross-section incidence rate indicates that the cross-sectional shape of the fiber is abnormal. This is a value indicating the proportion (%) of filaments. In order to determine whether the fiber cross section is abnormal, the fiber cross section was observed under a microscope, and a filament with three or less concave portions and three or less convex portions was determined to be a filament with an abnormal fiber cross section.
【表】【table】
【表】
実施例 2
メタノール比が12重量%である塩化メチレンと
メタノールとの混合物にセルロースジアセテート
とその濃度が22重量パーセントとなるように溶解
させた溶液を通常どおりに過して紡糸原液と
し、この紡糸原液を第2表に示す温度に加熱した
後にVT/VE比が0.85以下でかつ0.80以上となるよ
うに選んだ紡糸ノズルから吐出させ、通常の方法
で乾燥して800m/分の速度で引き取り、100デニ
ール27フイラメントのアセテート繊維を得、その
結果を第2表に示した。[Table] Example 2 A solution of cellulose diacetate dissolved in a mixture of methylene chloride and methanol with a methanol ratio of 12% by weight to a concentration of 22% by weight was filtered as usual to obtain a spinning stock solution. After heating this spinning stock solution to the temperature shown in Table 2, it was discharged from a spinning nozzle selected so that the V T /V E ratio was 0.85 or less and 0.80 or more, and dried in the usual manner at 800 m/min. The results are shown in Table 2.
【表】
実施例 3
メタノール比が12重量%である塩化メチレンと
メタノールとの混合物にセルロースジアセテート
をその濃度が22重量パーセントとなるように溶解
させた溶液が通常どおりに過して紡糸原液と
し、この紡糸原液をノズル孔直径が37μから41μ
である紡糸ノズルから吐出させ通常どおりに乾燥
して800m/分の速度で引き取り、100デニール27
フイラメントのアセテート繊維を得、その結果を
第3表に示した。[Table] Example 3 A solution of cellulose diacetate dissolved in a mixture of methylene chloride and methanol with a methanol ratio of 12% by weight to a concentration of 22% by weight was filtered as usual to obtain a spinning stock solution. , this spinning stock solution is applied to a nozzle hole with a diameter of 37μ to 41μ.
It is spun out from a spinning nozzle, dried as usual, and taken up at a speed of 800 m/min to produce 100 denier 27
Filament acetate fibers were obtained and the results are shown in Table 3.
Claims (1)
タノールとの混合物からなり、この混合物中のメ
タノールの割合が8〜15重量%である有機溶媒に
セルロースジアセテートの濃度が21〜24重量%に
なるように溶解して紡糸原液となし、この紡糸原
液を70〜80℃に加熱した後、VT/VE(但し、VE
は紡糸原液の紡糸ノズルからの吐出速度、VTは
糸条の引き取り速度を示す)が0.85〜0.80となる
条件下で乾式紡糸することを特徴とするアセテー
ト繊維の製造方法。1 Cellulose diacetate is dissolved in an organic solvent consisting of a mixture of methylene chloride and methanol in which the proportion of methanol in the mixture is 8 to 15% by weight so that the concentration of cellulose diacetate is 21 to 24% by weight. After heating this spinning stock solution to 70-80℃, V T /V E (however, V E
1. A method for producing acetate fibers, which comprises performing dry spinning under conditions such that a spinning dope is discharged from a spinning nozzle at a speed of 0.85 to 0.80 ( VT is a yarn take-up speed).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4173482A JPS58163716A (en) | 1982-03-18 | 1982-03-18 | Preparation of acetate fiber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4173482A JPS58163716A (en) | 1982-03-18 | 1982-03-18 | Preparation of acetate fiber |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS58163716A JPS58163716A (en) | 1983-09-28 |
JPH0229764B2 true JPH0229764B2 (en) | 1990-07-02 |
Family
ID=12616646
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4173482A Granted JPS58163716A (en) | 1982-03-18 | 1982-03-18 | Preparation of acetate fiber |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS58163716A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0717561U (en) * | 1993-07-08 | 1995-03-28 | 勲 山本 | Birthday calendar |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6099002A (en) * | 1983-10-31 | 1985-06-01 | Mitsubishi Acetate Co Ltd | Preparation of acetate yarn |
JPS60194108A (en) * | 1984-03-12 | 1985-10-02 | Mitsubishi Acetate Co Ltd | Manufacture of diacetate fiber |
-
1982
- 1982-03-18 JP JP4173482A patent/JPS58163716A/en active Granted
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0717561U (en) * | 1993-07-08 | 1995-03-28 | 勲 山本 | Birthday calendar |
Also Published As
Publication number | Publication date |
---|---|
JPS58163716A (en) | 1983-09-28 |
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