KR0160467B1 - Method for manufacturing artificial leather - Google Patents
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- KR0160467B1 KR0160467B1 KR1019930020859A KR930020859A KR0160467B1 KR 0160467 B1 KR0160467 B1 KR 0160467B1 KR 1019930020859 A KR1019930020859 A KR 1019930020859A KR 930020859 A KR930020859 A KR 930020859A KR 0160467 B1 KR0160467 B1 KR 0160467B1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Polyurethanes Or Polyureas (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
본 발명은 인공피혁의 제조방법으로 최종 단사섬도가 0.3데니어 이하인 극세사로 제조된 기포를 유기디이소시아네이트, 폴리테트라메틸렌글리콜, 질소원자 미함유 저분자 디올, 질소원자 함유 저분자 디올, 고분자 트리올 및 디메틸포름아마이드를 사용하여 제조된 폴리우레탄에 함침시킨후 버핑, 함금염료 사용염색, 버핑, 소핑등 일련의 후가공 처리를 행함을 특징으로한 인공피혁의 제조방법이며 내가수분해성 및 염색성이 우수하여 고급 의료용 및 각종 잡화용 소재로 유용한 인공피혁을 제공한다.The present invention is a method of manufacturing artificial leather, the final single yarn fineness of 0.3 denier or less microfiber filament is produced by the organic diisocyanate, polytetramethylene glycol, nitrogen atom-free low molecular diol, nitrogen atom-containing low molecular diol, polymer triol and dimethylform It is a manufacturing method of artificial leather characterized by performing a series of post-processing treatments such as buffing, dyeing using dye dye, buffing, soaping after impregnating polyurethane manufactured using amide. Provides artificial leather which is useful for various miscellaneous materials.
Description
본 발명은 내가수분해성 및 염색성이 우수한 인공피혁의 제조방법에 관한 것이다.The present invention relates to a method for producing artificial leather excellent in hydrolysis resistance and dyeing.
좀더 상세하게는 극세사로된 기포에 유기디이소시아네이트, 폴리테트라메틸렌글리콜, 질소원자 미함유 저분자 디올, 질소원자 함유 저분자 디올, 고분자 트리올 및 디메틸포름아마이드를 사용하여 제조된 폴리우레탄에 함침시킨후 버핑 염색등 후가공 처리를 진행하여 내가수분해성과 염색성이 우수한 인공피혁의 제조방법에 관한 것이다.More specifically, microfiber bubbles are impregnated with polyurethane prepared using organic diisocyanate, polytetramethylene glycol, low molecular weight diol containing no nitrogen atom, low molecular weight diol containing nitrogen atom, high molecular triol and dimethylformamide, and buffing. The present invention relates to a method for producing artificial leather having excellent hydrolysis resistance and dyeing property by performing post-processing treatment such as dyeing.
인공피혁은 코팅대상기포에 고분자 탄성체를 충진시킨후 염색, 버핑등 다양한 후가공을 통해 제조되는데 충진된 고분자 탄성체의 염색에 큰 어려움을 갖고 있어 이의 해결에 다양한 연구가 시도되고 있다.Artificial leather is manufactured through various post-processing such as dyeing and buffing after filling a polymeric elastomer with a coating fabric. Various researches have been attempted to solve the problem because of the great difficulty in dyeing the filled polymeric elastomer.
인공피혁 제조에 사용되는 고분자 탄성체로는 폴리우레탄이 주로 사용되는데 일반적인 방법으로 제조된 폴리우레탄은 염색이 잘 되지 않고 알칼리에 취약하여 내가수분해성이 불량한 문제점을 갖고 있다.Polyurethane is mainly used as a polymer elastic body used in the manufacture of artificial leather. Polyurethane prepared by a general method is not easily dyed and has a problem of poor hydrolysis resistance because it is vulnerable to alkali.
폴리우레탄의 염색성을 향상시키기 위한 방법으로는 1) 제 3급 질소원자를 폴리우레탄 중합쇄내에 도입하는 방법(일본 특허공고 제 62-23097), 2) 유기산 또는 무기산과 제3급 아민과의 염을 폴리우레탄 중합쇄중에 도입하는 방법(일본 특허공고 제 75-17520), 3) 폴리우레탄 중합쇄의 말단에 제3급 또는 제4급 질소원자를 도입하는 방법(일본특허 공고 제 69-16386)등이 제안되어 왔다. 그러나 방법 1)과 2)는 반응중 겔(Gel)이 형성되기 쉽고 방법 3)은 질소원자의 도입량을 제어하기 힘들고 탄성이 떨어지는 단점이 있었다.Methods for improving the dyeability of polyurethane include 1) introducing a tertiary nitrogen atom into the polyurethane polymer chain (Japanese Patent Publication No. 62-23097), 2) salts of organic or inorganic acids with tertiary amines. (3) Introduced into the polyurethane polymer chain (Japanese Patent Publication No. 75-17520), 3) A method of introducing a tertiary or quaternary nitrogen atom into the terminal of the polyurethane polymer chain (Japanese Patent Publication No. 69-16386) And the like have been proposed. However, Method 1) and 2) are easy to form gel during the reaction, and Method 3) has a disadvantage in that it is difficult to control the amount of nitrogen atoms introduced and the elasticity is poor.
또한 폴리우레탄을 안료에 의한 착색으로 색상을 부여하는 방법도 시도되고 있으나 염색견뢰도가 취약한 문제점이 있었다.In addition, a method of imparting a color by coloring the polyurethane with the pigment has been attempted, but there was a problem that the dye fastness is weak.
따라서 본 발명의 목적은 이와같은 종래의 문제점을 해결하기 위하여 안출된 것으로, 특수하게 조성된 폴리우레탄 수지를 코팅대상 기포에 함침시키고 염색, 버핑등 후처리 가공을 수행하는 것을 특징으로한 염색성이 우수하여 주농색 발현이 가능하고 견뢰도가 우수한 인공피혁을 제조하는 방법을 제공하는 것이다.Therefore, the object of the present invention was devised to solve such a conventional problem, and excellent dyeing characteristics, characterized in that the specially formulated polyurethane resin is impregnated in the coating target bubble and performing post-treatment such as dyeing, buffing. It is to provide a method for producing artificial leather capable of expressing the main color and excellent fastness.
본 발명에서는 특히 유기디이소시아네이트(A), 고분자 디올(B), 질소원자를 포함하지 않는 저분자 디올(C), 질소원자를 포함하는 저분자 디올(D), 고분자 트리올(E) 및 유기용매(F)를 포함하여 제조된 폴리우레탄을 사용하는 것을 특징으로 한다.In the present invention, organic diisocyanate (A), polymer diol (B), low molecular diol (C) containing no nitrogen atom, low molecular diol (D) containing nitrogen atom, high molecular triol (E) and organic solvent ( It is characterized by using a polyurethane prepared, including F).
본 발명에 사용되는 코팅대상 기포로는 일반적인 인공피혁 제조에 사용되는 모든 기포가 가능하나 유연성이 우수한 인공피혁을 제조하기 위해서는 최종 단사섬도가 0.3데니어 이하의 극세사로 제조된 직포, 트리코트지, 부직포등이 적합하며, 특히 최종 인공피혁의 물성이 우수한 강점으로 인해 부직포가 가장 바람직하다.As the bubble to be coated in the present invention, all bubbles used in general artificial leather can be manufactured, but in order to manufacture artificial leather having excellent flexibility, the final single yarn fineness is made of microfibers having 0.3 denier or less, woven fabric, tricot paper, and nonwoven fabric. Etc. are suitable, and nonwoven fabrics are most preferred because of the excellent strength of the final artificial leather.
이러한 부직포로는 예를 들면 카딩이 가능한 2-6데니어의 섬유형성 성분과 가용성 성분으로 이루어진 복합섬유를 밀도 0.20g/㎤ 이상으로 니들펀치(Needle-punch)한 부직포를 들수있다. 이러한 복합섬유 부직포 시이트를 함침하는 고분자 탄성체로서 본 발명에서 특징적으로 사용하는 폴리우레탄은 상술한 바와같이 성분(A)∼(E)를 유기용매(F)와 함께 혼합반응 시켜 수득하는 것으로, 여기에서 상기 유기디이소시아네이트(A)로는 4,4'-디페닐메탄 디이소시아네이트, 1-6-헥사메틸렌 디이소시아네이트, 이소포론 디이소시아네이트중에서 선택된 1종을 3내지 9중량%로 사용하는 것이 좋고, 상기 고분자 디올(B)성분으로는 에테르계 디올을 사용하되 분자량 1,500∼2,000사이의 폴리테트라메틸렌글리콜을 10내지 30중량%로 선택적으로 사용하는 것이 좋고, 상기 질소원자 미함유 저분자 디올(C) 성분으로는 1,6-헥산디올을 0.5내지 2.5중량%로 사용하는 것이 바람직하며, 상기 질소원자 함유 저분자 디올(D)성분으로는 N-메틸디에탄올아민을 0.05내지 0.35중량%로 사용하는 것이 바람직하고, 상기 고분자 트리올(E) 성분으로는 폴리프로필렌트리올을 0.5내지 2.0중량%로 사용하는 것이 바람직하며, 상기 유기용매(F)로는 디메틸포름아마이드를 사용하는 것이 좋다.Examples of such nonwoven fabrics include needle-punched nonwoven fabrics having a density of 0.20 g / cm 3 or more of a composite fiber composed of 2-6 denier fiber-forming components and soluble components. As a polymer elastic body impregnating such a composite fiber nonwoven sheet, the polyurethanes characteristically used in the present invention are obtained by mixing components (A) to (E) with an organic solvent (F) as described above. As the organic diisocyanate (A), it is preferable to use 3 to 9% by weight of one selected from 4,4'-diphenylmethane diisocyanate, 1-6-hexamethylene diisocyanate and isophorone diisocyanate. As the diol (B) component, it is preferable to use an ether-based diol, but selectively use 10 to 30% by weight of polytetramethylene glycol having a molecular weight of 1,500 to 2,000, and the nitrogen-free low molecular diol (C) component It is preferable to use 1,6-hexanediol at 0.5 to 2.5% by weight, and as the nitrogen atom-containing low molecular diol (D) component, N-methyldiethanolamine is contained in 0.05 to 0.35. It is preferable to use in%, the polymer triol (E) component is preferably 0.5 to 2.0% by weight of polypropylene triol, the dimethyl formamide is preferably used as the organic solvent (F). .
본 발명의 폴리우레탄 제조에 있어서 특히 질소원자 함유 저분자 디올(D)로서는 두히드록시기를 직접 연결하는 쇄내에 존재하는 탄소의 갯수가 2개이상이고, 질소원자에 연결된 세개의 기중 하나 또는 두개가 메틸기인 것이 바람직한데, 이러한 구조의 저분자 디올로 N-부틸디에탄올아미, 3-피를리디오-1,2-프로판디올, 3-디메틸아미노-1,2-프로판디올등도 사용될 수 있으나, 연질성 면에서 우수한 N-메틸디에탄올아민을 선택하는 것이 좋다.In the production of the polyurethane of the present invention, in particular, the nitrogen atom-containing low molecular diol (D) is two or more carbons present in the chain directly connecting two hydroxy groups, and one or two of the three groups linked to the nitrogen atom is a methyl group. It is preferable to use N-butyl diethanolami, 3-pyridio-1,2-propanediol, 3-dimethylamino-1,2-propanediol and the like as the low molecular weight diol of such a structure. It is good to select N-methyldiethanolamine which is excellent in terms.
또한 N-메틸디에탄올아민은 전체조성물에 대해 상술한 바와같이 0.05내지 0.35중량%로 사용하는 것이 좋은데, 0.05중량% 이하이면 염색성 향상의 효과가 없고 0.35중량% 이상이면 탄성이 저하되기 때문이다. 본 발명에서 상술한 성분(A)∼(F)로부터 폴리우레탄을 중합하는 방법으로서는 유기디이소시아네이트(A)와 고분자 디올(B), 저분자 디올(C,D), 고분자 트리올(E)을 초기에 모두 투입하고 반응을 진행시키는 원숏법을 사용하는 것이 바람직하다.In addition, N-methyldiethanolamine is preferably used at 0.05 to 0.35% by weight as described above with respect to the entire composition, since 0.05% by weight or less does not have an effect of improving dyeing property, and 0.35% or more by weight reduces elasticity. As a method of polymerizing a polyurethane from the above-mentioned components (A)-(F) in this invention, organic diisocyanate (A), high molecular diol (B), low molecular diol (C, D), and high molecular triol (E) are initial stages. It is preferable to use the one-shot method which adds all to the process and advances reaction.
유기 디이소시아네이트(A)와 고분자 디올(B)을 먼저 반응시키고 난후 생성된 프리폴리머를 저분자 디올(C,D)과 잔량의 유기 디이소시아네이트(A)와 함께 다시 반응시키는 프리폴리머법을 사용할 경우, 원숏법으로 반응시켰을때보다 염색성 및 탄성이 떨어진다. 또한 반응을 진행시킬때의 온도는 60℃∼90℃로 유지하는 것이 바람직한데, 이에서 벗어날 경우 반응이 충분히 진행되지 않거나 원료의 물성이 떨어지게 된다.In the case of using a prepolymer method in which an organic diisocyanate (A) and a polymer diol (B) are reacted first, and then a prepolymer produced is reacted again with a low molecular diol (C, D) and a residual organic diisocyanate (A), a one-shot method. Dyeability and elasticity is lower than when reacted with. In addition, it is preferable to keep the temperature at 60 ° C to 90 ° C when the reaction proceeds. If this occurs, the reaction does not proceed sufficiently or the physical properties of the raw material are deteriorated.
상기한 방법으로 제조된 폴리우레탄은 인공피혁 제조에 적합한 수준의 내가수분해성 및 연질성을 가지면서 염색성이 우수하여 농색발현이 가능한 장점이 있다.Polyurethane prepared by the above method has the advantage of being capable of deep color expression with excellent dyeability while having hydrolysis resistance and softness of a level suitable for artificial leather production.
상기 폴리우레탄에 함침된 피혁상 시이트를 240-320메쉬의 샌트페이퍼로 버핑하고 액류염색기에서 함금염료를 사용하여 염색한후, 320-400메쉬의 샌드페이퍼로 후처리 버핑을 한다.The leather-impregnated sheet impregnated with the polyurethane is buffed with 240-320 mesh sandpaper and dyed using a dye dye in a liquid dyeing machine, followed by post-processing buffing with sandpaper of 320-400 mesh.
이렇게 하여 제조된 시이트를 액류염색기에서 소핑(Soaping)한후 모미 가공 및 표면 정리가공을 하여주면 유연하고 염색성이 우수하여 농색을 발현하는 염색견리도가 우수한 인공피혁을 얻을 수 있다. 이렇게 제조된 인공피혁은 염색성이 우수한 폴리우레탄을 사용하여 후가공을 진행하기 때문에 농색 발현이 가능하고 염색견뢰도가 우수하여 고급 의료용 및 각종 잡화용 소재로 사용될 수 있고 내가수분해성과 소프트니스가 우수하기 때문에 신발 갑피용 소재로의 사용이 가능하다.The sheet thus prepared is soaped in a liquid dyeing machine, and then subjected to Momi processing and surface finishing, thereby obtaining artificial leather having excellent dyeing degree, which is soft and excellent in dyeing. The artificial leather manufactured in this way can be used for high-quality medical and various miscellaneous materials because of its deep dyeing and excellent dyeing fastness because it uses post-processing polyurethane using excellent dyeing property, and it has excellent hydrolysis resistance and softness. It can be used as a material for shoe uppers.
[실시예 1]Example 1
테레프탈산 대비 4몰%의 5소디움설포이소프탈산으로 공중합된 폴리에스터 해성분과 나일론 6 도성분을 도수 36본/필라멘트 복합비 35:65로 복합방사한 다음 크림프수 16개/인치, 3데니어, 51mm인 스태플 파이버를 얻었다.The polyester sea component copolymerized with 4 mole% 5 sodium sulfoisophthalic acid and 6 nylon degree components of terephthalic acid was spun at a combined 36 / filament ratio of 35:65, and then the number of crimps was 16 / inch, 3 denier, and 51 mm. Got staple fiber.
상기 스태플 파이버를 카딩하고 통상의 방법으로 크로스래핑한후 니들펀칭을 거쳐 중량이 320g/㎡인 방향성이 없는 두께 1.4mm, 겉보기 밀도 0.23g/㎤인 부직포를 제조하였다.The staple fiber was carded and cross-wrapped in a conventional manner, and then needle punched to produce a nonwoven fabric having a non-directional thickness of 1.4 mm and an apparent density of 0.23 g / cm 3 with a weight of 320 g / m 2.
상기 복합섬유 부직포 시이트에 100% 모듈러스 24kg/㎠인 폴리우레탄을 함침시켜 피혁상 시이트를 제조하였다.Leather composite sheets were prepared by impregnating the composite fiber nonwoven sheet with 100% modulus of 24 kg / cm 2 polyurethane.
함침한 폴리우레탄을 4,4'-디페닐메탄 이소시아네이트 6.4중량%, 분자량 2000의 폴리테트라 메틸렌글리콜 20.8중량%, 탄소 6개의 1,6-헥산디올 1.5중량%, N-메틸디에탄올아민 0.2중량%, 분자량 3000의 폴리프로필렌트리올 1.1중량%을 원료로하여 용매인 4,4'-디메틸포름아마이드 70중량% 존재하여 원숏법으로 제조한 것이다.6.4 wt% of 4,4'-diphenylmethane isocyanate, 20.8 wt% of polytetra methylene glycol having a molecular weight of 2000, 1.5 wt% of 1,6-hexanediol of 6 carbons, 0.2 wt% of N-methyldiethanolamine % And 1.1% by weight of polypropylenetriol having a molecular weight of 3000 were used as a raw material and 70% by weight of 4,4'-dimethylformamide as a solvent was prepared by the one-shot method.
상기 시이트를 물 90부, DMF 10부로된 응고조에서 습식 응고하고 70℃ 온수에서 수세, 건조후 가성소다 2%농도, 온두 95℃의 욕중에서 공중합 폴리에스터를 완전감량 제거한 후 건조하였다. 건조된 시이트를 노즐직경 0.2mm, 수압 60kg/㎠인 고압수류존을 통과시켜 건조시킨 다음 320메쉬의 샌드페이퍼로 버핑하고 액류염색기에서 함금염료를 사용하여 염색한후 400메쉬의 샌드페이퍼로 후처리 버핑하여 피혁상 시이트를 제조하였다. 이렇게 제조된 시이트를 액류염색기에서 소핑(Soaping)한후 모미가공 및 표면 정리가공을 하여 인공피혁을 제조하였다.The sheet was wet-coagulated in a coagulation bath consisting of 90 parts of water and 10 parts of DMF, washed with hot water at 70 ° C., dried, and completely dried after removing the copolyester in a bath of 2% concentration of caustic soda and 95 ° C. in hot water. The dried sheet was dried through a high pressure water flow zone having a nozzle diameter of 0.2 mm and a water pressure of 60 kg / cm 2, then buffed with 320 mesh sandpaper, dyed with an alloy dye in a liquid dyeing machine, and then post-treated with 400 mesh sand paper. The leather sheet was produced. The sheet thus prepared was soaped in a liquid dyeing machine, and then artificial leather was prepared by processing and surface finishing.
[실시예 2]Example 2
복합섬유의 도수가 19본/필라멘트인 것을 사용하고 2.5데니어, 45mm, 22 크림프/인치인 스태플 파이버를 제조하여 실시예 1과 동일하게 인공피혁을 제조하였다.Synthetic fibers were manufactured in the same manner as in Example 1 by using a staple fiber having a frequency of 19 fibers / filament and using 2.5 denier, 45 mm, and 22 crimp / inch.
[비교예 1]Comparative Example 1
함침되는 폴리우레탄으로 4,4'-디페닐 메탄 이소시아네이트를 6.4중량부, 에틸렌클리콜을 20.8중량부, 4,4'-디메틸포름아마이드를 70중량부로 하여 제조된 일반적인 폴리우레탄을 사용하는 것외에는 실시예 1과 동일하게 진행하였다.Except for using a general polyurethane prepared by impregnating polyurethane, 6.4 parts by weight of 4,4'-diphenyl methane isocyanate, 20.8 parts by weight of ethylene glycol, and 70 parts by weight of 4,4'-dimethylformamide. It proceeded similarly to Example 1.
[비교예 2]Comparative Example 2
함침되는 폴리우레탄제조에 있어서 유기 디이소이아네이트(A)와 고분자 디올(B)을 먼저 반응시키고난후 생성된 프리폴리머를 저분자 디올(C,D)와 반응시키는 프리폴리머법으로 제조하는 것외에는 실시예 1과 동일하게 진행하였다.In preparing the impregnated polyurethane, except that the organic diisoyanate (A) and the polymer diol (B) are first reacted, and then the prepolymer produced is reacted with the low molecular diol (C, D) to prepare a prepolymer method. Proceed as in the following.
[비교예 3]Comparative Example 3
질소원자 미함유 저분자 디올(탄소 6개의 1,6-헥산디올)을 1.3중량%, 질소원자함유 저분자 디올(N-메틸디에탄올아민)를 0.4% 사용한 것외에는 실시예 1과 동일하게 진행하였다.The procedure was the same as in Example 1 except that 1.3% by weight of the nitrogen-free low molecular diol (6 carbon 6,6-hexanediol) and 0.4% of the nitrogen atom-containing low molecular diol (N-methyldiethanolamine) were used.
비교를 위하여 상기 실시예 및 비교예에 의하여 제조된 인공피혁의 특성을 표 1에 나타내었다.Table 1 shows the characteristics of the artificial leather produced by the above Examples and Comparative Examples for comparison.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101049185B1 (en) * | 2007-02-26 | 2011-07-14 | 코오롱인더스트리 주식회사 | Artificial leather with excellent elasticity and its manufacturing method |
WO2013187607A1 (en) * | 2012-06-12 | 2013-12-19 | 한국생산기술연구원 | Fiber treatment agent for cotton fiber knitted fabric and cotton fiber knitted fabric treated with the treatment agent |
KR101400679B1 (en) * | 2007-05-02 | 2014-05-29 | 주식회사 영풍필텍스 | Coating Material for High Tension Protecting Fabric and Manufacturing Method Therefor |
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1993
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101049185B1 (en) * | 2007-02-26 | 2011-07-14 | 코오롱인더스트리 주식회사 | Artificial leather with excellent elasticity and its manufacturing method |
KR101400679B1 (en) * | 2007-05-02 | 2014-05-29 | 주식회사 영풍필텍스 | Coating Material for High Tension Protecting Fabric and Manufacturing Method Therefor |
WO2013187607A1 (en) * | 2012-06-12 | 2013-12-19 | 한국생산기술연구원 | Fiber treatment agent for cotton fiber knitted fabric and cotton fiber knitted fabric treated with the treatment agent |
KR101368825B1 (en) * | 2012-06-12 | 2014-03-03 | 한국생산기술연구원 | Treatment agent for cotton knitting textile and the knitting textile treated therewith |
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