KR920008976B1 - Process for the production of polyester conjugated fibers - Google Patents
Process for the production of polyester conjugated fibers Download PDFInfo
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- KR920008976B1 KR920008976B1 KR1019900011488A KR900011488A KR920008976B1 KR 920008976 B1 KR920008976 B1 KR 920008976B1 KR 1019900011488 A KR1019900011488 A KR 1019900011488A KR 900011488 A KR900011488 A KR 900011488A KR 920008976 B1 KR920008976 B1 KR 920008976B1
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
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Abstract
Description
본 발명은 카치온염료 가염형 개질 폴리에스터 섬유의 제조방법중 카치온염료 가염형 폴리에스터와 일반 폴리에스터를 적합한 방사조건에서 시스-코아 복합방사하여 폴리우레탄으로 코팅할때 용제로 사용되는 디메틸 포름아마이드 처리시 강도저하가 적은 카치온염료 가염형 개질 폴리에스터의 제조방법이다.The present invention is a dimethyl formamide treatment which is used as a solvent when coating a polyurethane with a cis-coa composite spinning of a cationic dye salt type polyester and a general polyester in a suitable spinning condition in a method of producing a cationic dye salt type modified polyester fiber. It is a method for producing a cationic dye salt-modified polyester with low strength drop.
폴리에스터는 여러가지 우수한 특성을 갖고 있어 섬유, 필름등으로 사용영역이 확대되고 있으나, 분산염료 이외의 염료로는 염색이 곤란하다.Polyester has various excellent properties, and its use area is expanded to fibers, films, etc., but dyeing with dyes other than disperse dyes is difficult.
그런데 폴리에스터 직물을 폴리우레탄으로 코팅하려할때 용제로 사용하는 디메틸 포름아마이드를 분산염료로 염색된 폴리에스터에 처리하면 디메틸 포름아마이드가 폴리에스터내에 존재하는 분산염료를 용출시키는 성질을 갖고있어 폴리에스터 직물은 폴리우레탄코팅에 제한을 받아왔다.However, when the polyester fabric is coated with polyurethane, dimethyl formamide, which is used as a solvent, is treated with a polyester dyed with a disperse dye, and dimethyl formamide dissolves the disperse dyes present in the polyester. Fabrics have been limited to polyurethane coatings.
그러나 카치온염료 가염형 개질 폴리에스터는 그 분자내에 카치온 염료와 강한 이온결합을 할 수 있는 극성기를 도입하고 있어, 카치온염료로 염색된 후 디메틸 포름아마이드를 처리하여도 염료가 용출되지 않는 장점을 가지고 있다. 반면에 카치온 염료 가염형 폴리에스터를 디메틸 포름아마이드로 처리했을때 일반 폴리에스터보다 강도저하가 심하여 일반 코팅직물로 사용하기에는 어려움이 있었다.However, since the cationic dye salt-type modified polyester has a polar group capable of strong ionic bonds with the cationic dye in its molecule, the dye does not elute even if the dimethyl formamide is treated after dyeing with the cationic dye. . On the other hand, when the cationic dye salted polyester is treated with dimethyl formamide, the strength is lower than that of general polyester, and thus it is difficult to use it as a general coating fabric.
상기 문제점을 해결하기 위한 본 발명은 카치온염료 가염형 폴리에스터를 시스성분으로 하고 일반 폴리에스터를 코아성분으로 복합방사하여 코아성분이 디메틸 포름아마이드 처리시 섬유의 강도저하를 방지하는 역할을 담당하는 점이 특징이다.The present invention for solving the above problems is that the composite component of the cationic dye salt-type polyester as the cis component and the common polyester as a core component to play a role in preventing the strength of the fiber during the dimethyl formamide treatment. It is characteristic.
본 발명에서 사용되는 카치온 염료 가염형 폴리에스터는 하기식(1)과 같이 표현되는 술폰산 금속염을 함유하는 이소프탈산성분을 1.0~7.0중량% 첨가된 수평균분자량 13,000~16,000의 개질 폴리에스터를 사용하며, 코아성분으로는 수평균분자량 18,000~25,000의 일반 폴리에스터를 사용한다.The cationic dye salt-type polyester used in the present invention uses a modified polyester having a number average molecular weight of 13,000 to 16,000 with an isophthalic acid component containing 1.0 to 7.0 wt% of a sulfonic acid metal salt represented by the following formula (1). As the core component, a general polyester with a number average molecular weight of 18,000 to 25,000 is used.
(단, M : 알칼리금속 또는 알칼리 토류금속 R,R' : 수소 또는 탄소수 1~20의 에스테르 형성성 치환체)(However, M: alkali metal or alkaline earth metal R, R ': hydrogen or ester-forming substituent of 1 to 20 carbon atoms)
본 발명에서 언급하고 있는 섬유횡단면의 시스성분과 코아성분은 그림 1에서 나타나 있듯이 섬유횡단면의 중심부를 코아성분이라 하고 외각성분을 시스성분이라 한다.The cis component and core component of the cross sectional fiber referred to in the present invention are referred to as the core component of the fiber cross section, and the outer component is referred to as the cis component.
이때 시스성분은 섬유횡단면의 면적비율로 30~70%이고 나머지 면적부분은 코아성분으로서 섬유제조 공정이 양호하고 디메틸 포름아마이드처리시 강도저하가 적은 복합섬유를 제조할 수 있다.At this time, the sheath component is 30 to 70% by the area ratio of the cross section of the fiber, and the remaining area is the core component, and the fiber manufacturing process is good, and the dimethyl formamide treatment can produce a composite fiber with little strength decrease.
시스성분이 섬유횡단면의 30% 이하일 경우, 즉 코아성분이 섬유횡단면의 70% 이상을 차지할 경우, 코아성분이 섬유상에서 한쪽으로 치우치거나 섬유표면으로 돌출되는 현상이 발생하여 카치온염료 염색시 균일한 염색을 얻기 어렵게 된다.If the sheath component is less than 30% of the cross-section of the fiber, that is, the core component accounts for more than 70% of the cross-section of the fiber, the core component may deviate from one side of the fiber or protrude to the fiber surface, resulting in uniform dyeing of the cationic dye. Dyeing becomes difficult to obtain.
또 시스성분이 섬유횡단면의 면적비율로 70% 이상일 경우, 즉 코아성분이 30% 이하일 경우에는 방사시 코아성분이 섬유중심축에 자리잡기가 어려우며 디메틸 포름아마이드 처리시 강도저하가 크게된다.In addition, if the sheath component is 70% or more in the area ratio of the cross-sectional area of the fiber, that is, the core component is less than 30%, the core component is difficult to settle in the fiber center axis during spinning, and the strength decrease is greatly increased when the dimethyl formamide is treated.
시스성분으로 사용되는 사용되는 개질 폴리에스터에 투입되는 술폰산 금속염을 함유하는 이소프탈산의 양은 최종 복합섬유의 염색성에 큰 영향을 미치는데, 시스성분이 섬유횡단면의 면적비율로 30~70%일 경우 술폰산 금속염을 함유하는 이소프탈산의 함유량은 1.0~7.0중량%가 적당하나 더욱 좋기로는 2.5~5.5중량%의 범위로 투입하는 것이 최종 염색성에 좋은 효과를 나타낸다. 함유량이 1.0중량% 이하일 경우 염색성이 떨어지며, 7.0중량% 이상일 경우는 디메틸 포름아마이드 처리시 강도 저하가 크다.The amount of isophthalic acid containing sulfonic acid metal salt added to the modified polyester used as the cis component greatly affects the dyeability of the final composite fiber. When the cis component is 30 to 70% by the area ratio of the cross section of the fiber, the sulfonic acid is used. The content of isophthalic acid containing a metal salt is preferably 1.0 to 7.0% by weight, but more preferably, 2.5 to 5.5% by weight of the isophthalic acid shows a good effect on the final dyeability. When the content is 1.0% by weight or less, the dyeability is inferior, and when it is 7.0% by weight or more, the strength decreases greatly during dimethyl formamide treatment.
개질 폴리에스터의 수평균 분자량은 13,000~16,000수준이 적절하며, 13,000 이하일 경우 디메틸 포름아마이드 처리시 강도저하가 크며, 16,000 이상일 경우 섬유의 색상이 황화되는 현상이 발생한다.The number average molecular weight of the modified polyester is 13,000 ~ 16,000 level is appropriate, the strength is greatly reduced when dimethyl formamide treatment when 13,000 or less, and the color of the fiber is yellowed when 16,000 or more.
코아성분으로 사용되는 일반 폴리에스터는 전체 복합섬유의 물리적 성질(예를들면 인장강도, 신장도 등)에 영향을 미치고 또한 디메틸 포름아마이드 처리후의 강도저하를 감소시키는 기능을 가지므로 가급적 분자량이 높은 폴리에스터를 사용하는 것이 유리하다.General polyester used as a core component has a function of affecting the physical properties (eg tensile strength, elongation, etc.) of the entire composite fiber and reducing the strength decrease after dimethyl formamide treatment. It is advantageous to use esters.
그러나 분자량이 너무 높을 경우 방사공정성이 불량하여지므로 적정수준의 분자량을 갖는 폴리에스터를 사용하여야 한다.However, if the molecular weight is too high, the spinning processability is poor, so a polyester having an appropriate molecular weight should be used.
본 발명자들은 수차례의 실험을 거쳐 시스성분으로 수평균 분자량 13,000~16,000의 개질 폴리에스터와 코아성분으로 수평균분자량 18,000~25,000의 일반 폴리에스터를 사용하였을때 방사공정성이 가장 안정됨을 발견하였다.After several experiments, the inventors found that the spinning processability is most stable when using a modified polyester having a number average molecular weight of 13,000 to 16,000 as a cis component and a general polyester having a number average molecular weight of 18,000 to 25,000 as a core component.
코아 성분인 일반 폴리에스터의 수평균 분자량이 18,000 이하일 경우는 복합섬유의 강도가 낮고 디메틸 포름아마이드 처리시 강도저하가 크며, 25,000 이상일 경우 섬유제조 공정성이 불량하여 진다.If the number average molecular weight of the polyester, which is a core component, is 18,000 or less, the strength of the composite fiber is low, and the strength decreases upon dimethyl formamide treatment, and when 25,000 or more, the fiber manufacturing processability is poor.
본 발명과 같은 복합방사법에 의해 카치온염료 가염형 폴리에스터를 제조할 경우, 단독방사법에 의하여 제조된 개질 폴리에스터보다 물성이 우수하며, 염색성은 동일한 복합섬유를 만들수 있다. 또한 디메틸 포름아마이드 처리시 단독방사법에 의한 것보다 강도저하가 적어 폴리우레탄 코팅용 직물로 사용이 가능하다.When the cationic dye salt-type polyester is manufactured by the composite spinning method as in the present invention, physical properties are better than those of the modified polyester produced by the single spinning method, and dyeing properties can make the same composite fiber. In addition, the dimethyl formamide treatment has a lower strength than that of the single spinning method can be used as a polyurethane coating fabric.
이하 본 발명에 의한 효과를 실시예 및 비교예에 따라 설명하면 다음과 같다.Hereinafter, the effects of the present invention will be described according to Examples and Comparative Examples.
[실시예 1]Example 1
술폰산 금속염을 함유하는 이소프탈산 성분을 3.0중량% 함유한, 수평균 분자량 15,000의 개질 폴리에스를 시스성분으로하고 수평균 분자량 20,000의 일반 폴리에스터를 코아성분으로 하는 75D/36F의 시스성분과 코아성분의 횡단면 면적비가 50 : 50인 복합섬유를 제조하였다.A cis component and a core component of 75D / 36F containing 3.0 wt% of an isophthalic acid component containing a sulfonic acid metal salt as a cis component with a modified polyester having a number average molecular weight of 15,000 as a core component and a general polyester having a number average molecular weight of 20,000 as a core component. A composite fiber having a cross-sectional area ratio of 50:50 was prepared.
이 복합섬유를 카치온염료로 염색하여 단면을 현미경으로 관찰한 결과 시스성분만 염색되고 코아성분은 염색되지 않음을 확인하였다.The composite fiber was dyed with cationic dye and the cross section was observed under a microscope to confirm that only the cis component was dyed and the core component was not dyed.
또 이 복합섬유를 상온의 디메틸 포름아마이드에 30분간 침지시킨후 60℃의 물속에서 1시간 동안 방치한 다음 열풍건조(130℃)하여 처리전후의 사물성(絲物性)을 측정하고 표 1에 비교예와 함께 결과를 나타내었다.In addition, the composite fiber was immersed in dimethyl formamide at room temperature for 30 minutes, left in water at 60 ° C. for 1 hour, and then hot-air-dried (130 ° C.) to measure the physical properties before and after treatment and compared with Table 1. The results are shown with examples.
[실시예 2]Example 2
술폰산 금속염을 함유하는 이소프탈산 성분을 4.5중량% 함유한, 수평균 분자량 13,500의 개질 폴리에스터를 시스성분으로 하고 수평균 분자량 22,000의 일반 폴리에스터를 코아성분으로 하는 100D/24F의 시스성분과 코아성분의 횡단면 면적비가 40 : 60인 복합섬유를 제조하였다.A cis component and a core component of 100D / 24F containing 4.5 wt% of an isophthalic acid component containing a sulfonic acid metal salt as a cis component with a modified polyester having a number average molecular weight of 13,500 as a cis component and a common polyester having a number average molecular weight of 22,000 as a core component A composite fiber having a cross sectional area ratio of 40:60 was prepared.
이 복합섬유를 카치온 염료로 염색하여 단면을 현미경으로 관찰한 결과 시스성분만 염색되고 코아성분은 염색되지 않음을 확인하였다.Staining this composite fiber with a cationic dye and observing the cross section under a microscope confirmed that only the cis component was dyed and the core component was not dyed.
디메틸 포름아마이드 처리방법은 실시예 1과 동일하며 그 결과를 표 2에 비교예와 함께 나타내었다.Dimethyl formamide treatment method is the same as in Example 1 and the results are shown in Table 2 together with the comparative example.
[비교예 1]Comparative Example 1
술폰산 금속염을 함유하는 이소프탈산 성분을 3.0중량% 함유한, 수평균 분자량 15,000의 개질 폴리에스터를 단독방사하여 75D/36F인 섬유를 제조하였다.A fiber of 75D / 36F was prepared by single spinning a modified polyester having a number average molecular weight of 15,000 containing 3.0% by weight of an isophthalic acid component containing a sulfonic acid metal salt.
이 섬유를 카치온염료로 염색하여 단면을 현미경으로 관찰한 결과 섬유의 횡단면 전체가 염색됨을 확인하였다.The fiber was dyed with cationic dye and the cross section was observed under a microscope to confirm that the entire cross section of the fiber was dyed.
디메틸 포름아마이드 처리방법은 실시예 1과 동일하며 그 결과를 표 1에 실시예와 함께 나타내었다.Dimethyl formamide treatment method is the same as in Example 1 and the results are shown in Table 1 together with the examples.
[비교예 2]Comparative Example 2
술폰산 금속염을 함유하는 이소프탈산 성분을 4.5중량% 함유한, 수평균분자량 13,500의 개질 폴리에스터를 단독방사하여 100D/24F인 섬유를 제조하였다.A fiber of 100D / 24F was prepared by single spinning a modified polyester having a number average molecular weight of 13,500 containing 4.5% by weight of an isophthalic acid component containing a sulfonic acid metal salt.
이 섬유를 카치온 염료로 염색하여 단면을 현미경으로 관찰한 결과 섬유의 횡단면 전체가 염색됨을 확인하였다.The fiber was dyed with cationic dye and the cross section was observed under a microscope to confirm that the entire cross section of the fiber was dyed.
디메틸 포름아마이드 처리방법은 실시예 1과 동일하며 그 결과를 표 2에 실시예와 함께 나타내었다.Dimethyl formamide treatment method is the same as in Example 1 and the results are shown in Table 2 together with the examples.
[비교예 3]Comparative Example 3
술폰산 금속염을 함유하는 이소프탈산 성분을 3.0중량% 함유한, 수평균분자량 15,000의 개질 폴리에스터를 시스성분으로 하고 수평균 분자량 20,000의 일반 폴리에스터를 코아성분으로 하는 75D/36F인 시스성분과 코아성분의 횡단면 면적비가 75 : 25인 복합섬유(비교예 3-1)와 면적비가 25 : 75인 복합섬유(비교예 3-2)를 제조하였다.A cis component and a core component of 75D / 36F containing 3.0 wt% of an isophthalic acid component containing a sulfonic acid metal salt as a cis component with a modified polyester having a number average molecular weight of 15,000 as a core component and a general polyester having a number average molecular weight of 20,000 as a core component A composite fiber having a cross-sectional area ratio of 75:25 (Comparative Example 3-1) and a composite fiber having an area ratio of 25:75 (Comparative Example 3-2) were prepared.
이 복합섬유를 카치온 염료로 염색하여 단면을 현미경으로 관찰한 결과 시스성분만 염색되고 코아성분은 염색되지 않음을 확인하였다.Staining this composite fiber with a cationic dye and observing the cross section under a microscope confirmed that only the cis component was dyed and the core component was not dyed.
디메틸 포름아마이드 처리방법은 실시예 1과 동일하며 그 결과를 표 3에 나타내었다.Dimethyl formamide treatment method is the same as in Example 1 and the results are shown in Table 3.
표 3에 나타나 있는 것과 같이 시스성분이 너무 많거나 너무 적으면 인장강도와 염색성을 동시에 만족시킬 수가 없다.As shown in Table 3, if the sheath component is too much or too little, the tensile strength and the dyeability cannot be satisfied at the same time.
[비교예 4][Comparative Example 4]
수평균분자량 20,000의 일반 폴리에스터를 단독방사하여 75D/36F인 섬유를 제조하였다.A fiber of 75D / 36F was prepared by single spinning a general polyester having a number average molecular weight of 20,000.
이 섬유를 분산 염료로 염색하여 단면을 현미경으로 관찰한 결과 섬유의 횡단면 전체가 염색됨을 확인하였다.The fiber was dyed with a disperse dye and the cross section was observed under a microscope to confirm that the entire cross section of the fiber was dyed.
또 이 섬유를 디메틸 포름아마이드에 30분간 침지시킨 후 60℃의 물속에서 1시간동안 방치한 다음 열풍 건조하여 처리전후의 사물성을 측정하고 표 4에 결과를 나타내었다.In addition, the fibers were immersed in dimethyl formamide for 30 minutes, left in water at 60 ° C. for 1 hour, and then dried by hot air to measure the physical properties before and after treatment, and the results are shown in Table 4.
표 4에서 알 수 있듯이 디메틸 포름아마이드(DMF) 처리시 분산염료가 용출되어 우레탄 코팅이 불가함을 알 수 있다.As can be seen from Table 4 it can be seen that the dispersion dye is eluted during the treatment of dimethyl formamide (DMF) is impossible urethane coating.
[표 1]TABLE 1
[표 2]TABLE 2
[표 3]TABLE 3
[표 4]TABLE 4
1) 표 1, 2에서 본 바와 같이 비교예 1, 2의 경우, 단독방사한 결과 디메틸 포름아마이드 처리시 강도저하가 심하다.1) As shown in Tables 1 and 2, in the case of Comparative Examples 1 and 2, the result of the single spinning resulted in a severe decrease in strength during dimethyl formamide treatment.
2) 염색조건은 다음과 같다.2) Dyeing conditions are as follows.
◎ 염료 투입량은 시료무게의 1.5중량%◎ Dye dose is 1.5% by weight of sample
◎ 염색욕조에 투입하는 물의 양은 시료무게의 50배◎ The amount of water added to the dye bath is 50 times the weight of the sample.
◎ 염색온도 : 120℃◎ Dyeing temperature: 120 ℃
◎ 염색시간 : 40분◎ Dyeing time: 40 minutes
3) 염료용출은 육안으로 판정하였다.3) Dye elution was visually determined.
4) 염착율은 다음과 같은 식에 의하여 구하였다.4) The dyeing rate was calculated by the following formula.
A : 염색욕조에 투입한 염료량(g)A: amount of dye added to the dye bath (g)
B : 염색후 욕조에 남아있는 염료량(g)B: amount of dye remaining in the bath after dyeing (g)
5) 강도유지율은 다음과 같은 식에 의하여 구하였다.5) Strength retention was calculated by the following equation.
A : DMF처리전의 강도(g/데니아)A: Strength before DMF treatment (g / denia)
B : DMF처리후의 강도(g/데니아)B: Strength after DMF treatment (g / denia)
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| KR20200009876A (en) * | 2018-07-20 | 2020-01-30 | 주식회사 휴비스 | Meta-Aramid Fiber improved dyeability |
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| KR20200009876A (en) * | 2018-07-20 | 2020-01-30 | 주식회사 휴비스 | Meta-Aramid Fiber improved dyeability |
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