KR100497908B1

KR100497908B1 - Making method therefor of dyeing of medicines

Info

Publication number: KR100497908B1
Application number: KR10-2002-0047248A
Authority: KR
Inventors: 김기준; 이명준; 이주엽
Original assignee: (주)대일화성
Priority date: 2002-08-09
Filing date: 2002-08-09
Publication date: 2005-06-29
Also published as: KR20040014077A

Abstract

본 발명은 염색시에 사용되는 염색조제의 제조방법에 관한 것으로, Oleylinidzolinim ethyl sulfate, 중수, 실리콘소포제,DETA, AEEA, 차아염소산, Alkylphosphate, EO를 질소하에서 혼합방응시켜 수지를 조성하는 수지조성과정과, 상기 수지 조성 과정에 의하여 제조된 수지, 과황산 나트륨, 디메틸설페이트, 메탄올과 에틸렌 옥사이드 혼합물, 아염소산 소다, 부틸셀로솔브를 질소하에서 혼합 교반 반응시켜 염색조제를 제조하는 염색 조제의 제조방법을 제공함으로써, 별도의 유연제와 이염제를 사용하지 않아도 되도록함과 아울러 피막의 두께가 안정되게 유지될 수 있는 정도의 열처리만으로 분산염료의 마이그레이션 방지와 함께 염색견뢰도가 우수한 심색가공을 할 수 있도록 한 것이다The present invention relates to a method for preparing a dyeing aid used during dyeing , comprising a resin composition process of forming a resin by mixing and reacting Oleylinidzolinim ethyl sulfate, heavy water, silicone antifoaming agent, DETA, AEEA, hypochlorous acid, Alkylphosphate, and EO under nitrogen. And a method of preparing a dyeing aid to prepare a dyeing aid by mixing and stirring a resin prepared by the resin composition process, sodium persulfate, dimethyl sulfate, methanol and ethylene oxide mixture, sodium chlorite, and butyl cellosolve under nitrogen. By providing a separate softener and dyeing agent, it is possible to prevent the migration of disperse dyes and to perform deep color processing with excellent color fastness by only heat treatment that can maintain the thickness of the film stably.

Description

Making method therefor of dyeing of medicines

본 발명은 염색시에 사용되는 염색조제의 제조방법에 관한 것으로, 보다 상세하게는 별도의 유연제와 이염제를 사용하지 않아도 되도록함과 아울러 피막의 두께가 안정되게 유지될 수 있는 정도의 열처리만으로 분산염료의 마이그레이션 방지와 함께 염색견뢰도가 우수한 심색가공을 할 수 있도록 하는 염색 조제의 제조방법에 관한 것이다.The present invention relates to a manufacturing method of a dyeing aid used during dyeing, and more particularly, it does not need to use a separate softening agent and a dyeing agent and is dispersed only by heat treatment to the extent that the thickness of the film can be stably maintained. The present invention relates to a manufacturing method of a dyeing assistant to prevent deep migration of dyes and to perform deep color processing with excellent dye fastnesses.

일반적인 염색방법은 윈치릴과 젯트노즐을 사용하여 직물을 고온고압상태의 염색조와 직물이송관을 통과시키면서 고압의 에어 또는 고온의 염액의 분사속도에 의해 가공이 이루어지게 되는데, 섬유가 고온 고압에 노출될 뿐 아니라 상기 젯트노즐과 윈치릴의 속도 불일치와 장시간 움직임으로인하여 섬유의 손상과 조직의 변화등이 발생되는 문제점이 있었다.In general dyeing method, the winch reel and the jet nozzle are used to process the fabric through the high speed and high pressure dye bath and the fabric conveying tube while the fabric is processed by the spraying speed of high pressure air or high temperature salt solution. As well as the jet nozzle and the winch reel due to the speed mismatch and the long-term movement, there was a problem that the damage of the fibers and changes in the tissue occurs.

그리고, 직접(直接) 염료로 침염 및 날염할시에는 흔히 세탁견뢰도가 만족스럽지 못한데, 예로써는 셀룰로오즈섬유 표면에 결합되어 있는 염료의 대부분이 세탁을 반복함에 따라 섬유로부터 이탈되며 세액으로 염료가 빠져나오면 염색되지 않았던 셀룰로오즈에 부분적으로 재흡착 할 수 있다.In addition, when dyeing and printing with direct dyes, washing fastness is often unsatisfactory. For example, most of the dyes bound to the surface of the cellulose fibers are released from the fibers as the washing is repeated, and when the dye comes out with the washing solution. Partially resorbed to cellulose that has not been stained.

이러한 단점들을 극복하기 위해서, 예를들면 섬유상에 금속염으로 착염화하거나, 섬유상에서 염료를 디아조화하거나 포름알데하이드로 염료 및/또는 섬유를 처리하거나, 인공수지에 함침시키거나, 양이온 보조제로 후처리하는 등의 많은 시도가이루어져 왔다. 양이온 후처리 보조제의 사용이 특히 효과적인 것으로 밝혀졌다.To overcome these shortcomings, for example, by complexing with metal salts on fibers, diazotizing dyes on fibers or treating formaldehyde dyes and / or fibers, impregnating artificial resins, or post-treatment with cationic aids. Many attempts have been made. The use of cationic workup aids has been found to be particularly effective.

상기한 모든 방법들은 견뢰도를 개선시키는 하지만, 그 결과가 일시적인 것이 단점이다. 양이온 후처리의 경우에도 반복세탁, 특히 알카리 상태하 50내지 100℃의 고온에서 반복세탁함으로써 보조제가 섬유로부터 이탈되며 이와 같이 양이온 보조제가 손실되면 개선된 습윤 견뢰도가 다시 소멸된다.All of the above methods improve the fastness, but the drawback is that the result is temporary. In the case of cationic post-treatment, the adjuvant is released from the fibers by repeated washing at high temperatures of 50 to 100 ° C. under alkaline conditions, and thus, the loss of the cationic adjuvant disappears again.

그리고, 반응성 염료 사용의 단점은 섬유에 화학적으로 결합되어 있는 염료는 수세견뢰도가 탁월하나, 염색후 잔류의 비고착 염료를 제거시키기 위해 직물을 완전히 세척하여야 하므로 수세견뢰도가 불량하게 되는 것이다.In addition, the disadvantage of using a reactive dye is that the dye chemically bonded to the fiber is excellent in water fastness, but the wash fastness is poor because the fabric must be thoroughly washed to remove the remaining non-fixed dye after dyeing.

또한, 종래의 염색조제에 의하면 멀링, 타링 또는 불균염 문제가 발생된다.In addition, according to the conventional dyeing aid, the problem of mulling, taring or disproportionate occurs.

상기한 바와 같은 문제점을 해결하기 우한 본 발명의 목적은 Oleylinidzolinim ethyl sulfate, 중수, 실리콘소포제,DETA, AEEA, 차아염소산, Alkylphosphate, EO를 질소하에서 혼합방응시켜 수지를 조성하는 수지조성과정과, 상기 수지 조성 과정에 의하여 제조된 수지, 과황산 나트륨, 디메틸설페이트, 메탄올과 에틸렌 옥사이드 혼합물, 아염소산 소다, 부틸셀로솔브를 질소하에서 혼합 교반 반응시켜 염색조제를 제조하여 별도의 유연제와 이염제를 사용하지 않아도 되도록함과 아울러 피막의 두께가 안정되게 유지될 수 있는 정도의 열처리만으로 분산염료의 마이그레이션 방지와 함께 염색견뢰도가 우수한 심색가공을 할 수 있도록 하는 염색 조제의 제조방법을 제공하는 데 있다.The object of the present invention to solve the above problems is a resin composition process for forming a resin by mixing and reacting Oleylinidzolinim ethyl sulfate, heavy water, silicone antifoaming agent, DETA, AEEA, hypochlorous acid, Alkylphosphate, EO under nitrogen, and the resin Resin, sodium persulfate, dimethylsulfate, methanol and ethylene oxide mixture, sodium chlorite, and butyl cellosolve were mixed and stirred under nitrogen to prepare dyeing aid. The present invention provides a method of preparing a dyeing aid that enables deep color processing with excellent dye fastness and prevention of migration of disperse dyes by only heat treatment to maintain the thickness of the film stably.

이와 같은 목적을 달성하기 위한 본 발명의 염색조제 제조방법을 하기에서 살펴본다.Looking at the dyeing preparation method of the present invention for achieving the above object.

우선 Oleylinidzolinim ethyl sulfate 5-40중량%와 중수 10-70중량%와 실리콘소포제 1-10중량%를 반응기에 투입 후 상온에서 질소를 투입하여 반응시키고 125-135℃로 승온시킨 후 DETA(Diethylene triamine) 5-30중량%를 서서히 투입하면서 125∼135℃를 유지하면서 30분 - 1시간동안 경과시키고, 175∼185℃로 승온시킨 후 그 온도를 유지하면서 3시간동안 반응시켜 9이하의 1차산가, 3급아민 6이하의 아민가, 연한 담황색 액상을 띄도록 한 후 95∼105℃로 냉각시키고, AEEA(Amino ethyl ethanol amine) 5-30중량%와 차아염소산 1-10중량%와 Alkylphosphate(대전 방지효과와 촉감 향상) 1-4중량%와 EO(ethylene Oxide) 5-40중량%를 95∼105℃에서 투입한 후 같은 온도에서 30분간 혼합하고 105∼115℃로 승온시킨 후 105∼115℃에서 1시간동안 탈수시킨 뒤 90∼100℃로 냉각시켜 수지를 조성한다.First, 5-40% by weight of Oleylinidzolinim ethyl sulfate, 10-70% by weight of heavy water, and 1-10% by weight of a silicone antifoam were added to the reactor, followed by reaction with nitrogen at room temperature, and then heated to 125-135 ° C. Then, DETA (Diethylene triamine) 5-30% by weight was gradually added while maintaining 125 to 135 ℃ 30 minutes-1 hour, and then heated to 175 ~ 185 ℃ and reacted for 3 hours while maintaining the temperature, the primary acid value of 9 or less, 3 Aqueous amines of 6 or less have a light pale yellow liquid, cooled to 95-105 ° C, 5-30% by weight of amino ethyl ethanol amine (AEEA), 1-10% by weight of hypochlorous acid, and Alkylphosphate (antistatic effect and Improved touch) 1-4% by weight and 5-40% by weight of EO (ethylene oxide) at 95-105 ℃, mixed at the same temperature for 30 minutes, heated to 105-115 ℃, and then heated at 105-115 ℃ for 1 hour. After dehydration for a while to cool to 90 ~ 100 ℃ to form a resin.

여기서 Oleyl imidazolinium 유도체로서 oleylimidasolinium ethyl sulpate는 섬유의 유연제, 양이온성이며, 섬유의 대전방지성과 구김현상을 현저하게 줄여준다.Oleylimidasolinium ethyl sulpate as an Oleyl imidazolinium derivative is a fabric softener, cationic, and significantly reduces the antistatic properties and wrinkles of the fiber.

그리고, 용매는 염색조제의 main product에 주로 사용되지만, 유연성, 재흡수성, 대전방지성, 구김현상을 줄여주는 1차 수지 합성 product만의 사용에도 가능하며 isopropyl alcohol:water = 1 : 1로 혼합하여 사용하고 이는 면, polyester, 아크릴 또는 혼방품에 적용 이들 염색물에 효과가 탁월하다.The solvent is mainly used for the main product of the dyeing aid, but it is also possible to use only the primary resin synthetic product which reduces flexibility, reabsorption, antistatic property and wrinkle phenomenon and is mixed with isopropyl alcohol: water = 1: 1. It is applied to cotton, polyester, acrylic or blends and is excellent for these dyeings.

상기한 바와 같은 공정에 의하여 제조된 수지 10-55중량%와 과황산 나트륨 5-30중량%를 반응조에 투입하여 상온에서 질소 투입한 후 2000-3000rpm속도로 교반하여 70-120℃로 승온시켜 디메틸설페이트 5-40중량%를 서서히 투입하면서 발열반응이 일어나도록 1-2시간동안 반응시킨 후 상온으로 냉각시키고, 메탄올과 에틸렌 옥사이드 혼합물 10-50중량%를 투입하여 pH는 5.5-6.8, 외관은 연황색 액상, 산가는 9 이하가 되도록 한 후, 과황산 나트륨 5-30중량%와 아염소산 소다 5-40중량%하여 탈색이 이루어지면 30분후에 부틸셀로솔브 10-50중량%와 과황산 나트륨 5-30중량%를 투입한다.10-55% by weight of the resin prepared by the above process and 5-30% by weight of sodium persulfate were added to the reactor, nitrogen was added at room temperature, stirred at 2000-3000 rpm, and heated to 70-120 ° C. to dimethyl. After slowly adding 5-40% by weight of sulfate to react for 1-2 hours to cause exothermic reaction, it was cooled to room temperature, and 10-50% by weight of methanol and ethylene oxide mixture was added to give a pH of 5.5-6.8. Yellow liquid, acid value of 9 or less, 5-30% by weight of sodium persulfate and 5-40% by weight of sodium chlorite, after 10 minutes of decolorization, 10-50% by weight of butyl cellosolve and sodium persulfate Add 5-30% by weight.

이와 같이 제조된 염색 조제는 피막의 두께가 안정되게 유지될 수 있는 정도의 열처리만으로 분산염료의 마이그레이션 방지와 함께 염색견뢰도가 우수한 심색가공을 할 수 있으며, 별도의 유연제를 이용한 가공이 필요없을 정도로 섬유에 유연성을 부여한다.The dyeing preparations prepared in this way can perform deep color processing with excellent dye fastness and prevent migration of disperse dyes only by heat treatment to the extent that the thickness of the film can be stably maintained, and the fiber does not need processing using a separate softening agent. Gives flexibility to

그리고, 본 발명의 염색 조제를 사용하여 이염제의 사용없이 폴리에스테르 섬유의 염색시 염색온도, 염착소요시간, 광견뢰도와 인열강도, 대전 방지성을 측정하여 표 1에 나타내며, 하기 표 1에서 알 수 있는 바와 같이 본 발명에 따른 염색 조제 제조 방법에 의하면 낮은온도이지만 광견뢰도와 인열강도, 대전방지성의 효과가 매우 우수함을 알 수 있다.In addition, by using the dyeing aid of the present invention to measure the dyeing temperature, dyeing time, light fastness and tear strength, antistatic properties when dyeing polyester fibers without using a dyeing agent is shown in Table 1, in Table 1 As can be seen, according to the method for preparing the dyeing preparation according to the present invention, it can be seen that the effect of light fastness, tear strength, and antistatic property is very excellent.

염색온도Dyeing temperature 염착소요시간Delay time 광견뢰도Light fastness 인열강도(gr)Tear strength (gr) 대전방지성Antistatic 종 래Species 130℃130 ℃ 35분35 minutes 불량Bad 12501250 불량Bad 본발명Invention 110℃110 ℃ 20분20 minutes 양호Good 16001600 양호Good

한편, 상기 표 1에서 인열강도는 엘멘도르프형 인열강도 측정기로, 대전방지성은 JIS L-0849에 따라 측정하였으며, 염색제품을 우레탄 포말로 보강하고 500시간 동안 페이드미터(fademeter)로 조사한 후에 그레이 스케일로 변색과 퇴색을 평가하였다.On the other hand, the tear strength in Table 1 was measured by Elmendorf type tear strength, the antistatic property was measured according to JIS L-0849, after reinforcing the dyeing product with urethane foam and irradiated with a fade meter for 500 hours Discoloration and fading were evaluated on a gray scale.

따라서, 본 발명에 따른 염색 조제의 제조방법에 의하면 섬유 직물의 깊은 색상과 유연성을 유지하기 위해 지나친 고열처리 보다는 피막의 두께가 안정되게 유지될 수 있는 정도의 열처리만으로 분산염료의 마이그레이션 방지와 함께 염색견뢰도가 우수한 심색가공을 할 수 있다.Therefore, according to the manufacturing method of the dyeing aid according to the present invention, in order to maintain the deep color and flexibility of the textile fabric, rather than excessive heat treatment, the thickness of the coating can be kept stable enough to prevent the migration of disperse dyes and dyeing together Deep color processing with excellent color fastness is possible.

또한, 섬유에 우수한 유연성을 가하므로 별도의 유연제를 이용한 가공이 필요없으며, 낮은온도에서 우수한 광견뢰도와 인열강도, 대전방지성의 효과를 얻을 수 있는 효과가 있다.In addition, since it adds excellent flexibility to the fiber, there is no need for processing using a separate softening agent, and it has an effect of obtaining excellent light fastness, tear strength, and antistatic property at low temperature.

그리고, 종래 침염에서 발생도는멀링 타링이나 불균염 문제가 해결되며, 우수한 제품을 생산하는데 생산성 향상과 윈치염색의 경우 수용된 섬유조직의 장시간 움직임에서 오는 섬유의 손상, 조직의 변화 등이 없는 효과가 있다.In addition, the incidence in conventional dyeing is solved the problem of the mulling tarring or disproportionate, and in producing an excellent product, there is no effect of improving the productivity and damage to the fiber resulting from long-term movement of the received fibrous tissue in the case of winch dyeing, tissue changes, etc. .

Claims

5-40% by weight of Oleylinidzolinim ethyl sulfate, 10-70% by weight of heavy water, and 1-10% by weight of silicone antifoam were added to the reactor and reacted by adding nitrogen at room temperature, and then heated to 125-135 ° C, followed by DETA (Diethylene triamine) 5 After 30 minutes-1 hour while slowly adding -30% by weight, maintaining 125 to 135 ℃, the temperature is raised to 175 ~ 185 ℃ and reacted for 3 hours while maintaining the temperature, the primary acid value of 9 or less, tertiary After amine 6 or less has a light pale yellow liquid, it is cooled to 95-105 ° C, and 5-30% by weight of amino ethyl ethanol amine (AEEA), 1-10% by weight of hypochlorous acid and 1-4% by weight of Alkylphosphate, 5-40% by weight of EO (ethylene oxide) at 95-105 ° C, mixed at the same temperature for 30 minutes, heated to 105-115 ° C, dehydrated at 105-115 ° C for 1 hour, and then at 90-100 ° C. A resin composition process of cooling the resin

10-55% by weight of the resin prepared by the above resin composition and 5-30% by weight of sodium persulfate were added to the reaction tank, nitrogen was added at room temperature, and stirred at 2000-3000 rpm to increase the temperature to 70-120 ° C., and then dimethyl sulfate. After slowly adding 5-40% by weight to react for 1-2 hours to generate an exothermic reaction, it is cooled to room temperature, and 10-50% by weight of a mixture of methanol and ethylene oxide is added. PH is 5.5-6.8 and the appearance is light yellow. After the liquid phase and acid value are 9 or less, 5-30% by weight of sodium persulfate and 5-40% by weight of sodium chlorite are decolorized, and after 30 minutes, 10-50% by weight of butyl cellosolve and 5% of sodium persulfate Method of producing a dyeing aid, characterized in that the -30% by weight.