KR101905888B1 - Manufacturing method of bath softner agent and bath softner agent manufactured by same method - Google Patents
Manufacturing method of bath softner agent and bath softner agent manufactured by same method Download PDFInfo
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- KR101905888B1 KR101905888B1 KR1020160105093A KR20160105093A KR101905888B1 KR 101905888 B1 KR101905888 B1 KR 101905888B1 KR 1020160105093 A KR1020160105093 A KR 1020160105093A KR 20160105093 A KR20160105093 A KR 20160105093A KR 101905888 B1 KR101905888 B1 KR 101905888B1
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- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 238000000034 method Methods 0.000 title abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000004902 Softening Agent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- -1 sodium sulfate alkyl ether Chemical class 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008213 purified water Substances 0.000 claims abstract description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 10
- 150000005215 alkyl ethers Chemical class 0.000 claims abstract description 10
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims abstract description 10
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 9
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 9
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 8
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 8
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 8
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 11
- 239000002979 fabric softener Substances 0.000 description 10
- 239000000835 fiber Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000003352 sequestering agent Substances 0.000 description 5
- 239000003599 detergent Substances 0.000 description 4
- 230000003405 preventing effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000037303 wrinkles Effects 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 3
- 229910010277 boron hydride Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical group 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004925 denaturation Methods 0.000 description 2
- 230000036425 denaturation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000021148 sequestering of metal ion Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000102 alkali metal hydride Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000004697 chelate complex Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000013077 scoring method Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- XFLNVMPCPRLYBE-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;tetrahydrate Chemical compound O.O.O.O.[Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O XFLNVMPCPRLYBE-UHFFFAOYSA-J 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
-
- C11D11/0017—
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/001—Softening compositions
- C11D3/0015—Softening compositions liquid
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/12—Soft surfaces, e.g. textile
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
본 발명은 정제수에 황산나트륨 알킬 에터, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터를 용해 및 혼합하는 1차 반응단계; 1차 반응단계에서 형성된 혼합물에 에틸렌디아민 테트라초산디나트륨, 에틸렌디아민 테트라초산테트라나트륨 및 소듐 벤조에이트를 첨가하고 나머지 정제수를 첨가하여 용해 및 혼합하는 2차 반응단계; 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계; 여과된 혼합물을 숙성시키는 숙성단계를 포함하는 욕중유연제의 제조방법 및 그 제조방법에 의하여 제조된 욕중유연제에 관한 것이다.The present invention relates to a process for producing a polyoxyethylene-polyoxypropylene alkyl ether, comprising: a first reaction step of dissolving and mixing a sodium sulfate alkyl ether and a polyoxyethylene-polyoxypropylene alkyl ether in purified water; A second reaction step in which disodium ethylenediaminetetraacetate, tetra sodium ethylenediamine tetraacetate and sodium benzoate are added to the mixture formed in the first reaction step and the remaining purified water is added to dissolve and mix; A filtration step of removing impurities from the mixture formed in the second reaction step; An aging step of aging the filtered mixture, and a bath softening agent produced by the method.
Description
본 발명은 욕중유연제의 제조방법 및 그 제조방법에 의한 욕중유연제에 관한 것으로 신규한 제조방법을 통해 구김 및 주름 방지 효과가 우수한 욕중유연제의 제조방법 및 그의 제조방법에 의한 욕중유연제에 관한 것이다.The present invention relates to a method for producing a bath softening agent and a bath softening agent by the method for producing the same, and a method for producing a bath softening agent excellent in wrinkling and wrinkle preventing effect through a novel manufacturing method and a bath softening agent by the method for producing the same.
일반적으로 섬유에 발생하는 꿉꿉한 냄새는 땀냄새 등의 성분인 유기화합물이 피부 상재균이 분해되어 생성된 불포화 저급 지방산 및 암모니아 등의 휘발성 유기화합물과 반응하거나 세탁세제 또는 섬유유연제 잔류성분과 반응하여 발생될 수 있다. 특히, 장마철의 경우, 실내 건조시 건조시간이 지연되므로 악취균인 Morxella asloensis로 인해 꿉꿉한 냄새가 더 발생하고 있는 것으로 알려졌다.Generally, the organic odor generated in fibers is caused by organic compounds such as sweat odor reacting with volatile organic compounds such as unsaturated lower fatty acids and ammonia formed by decomposition of the skin upright bacteria or reacting with laundry detergent or residues of fabric softener . Especially, in the case of rainy season, drying time is delayed during drying in the room, so it is known that odor is generated by Morxella asloensis, which is an odor bacterium.
이러한 꿉꿉한 냄새 등을 제거하기 위하여, 종래에는 항균제를 포함하는 섬유유연제 조성물을 사용했는데, 종래 섬유유연제에 포함되는 항균제는 인체에 유해하다는 내용이 보도됨에 따라 이러한 항균제의 사용이 최근에는 기피되고 있는 실정이다.Conventionally, a fabric softener composition containing an antibacterial agent has been used in order to remove such odor and the like. However, since it has been reported that the antibacterial agent contained in the conventional fabric softener is harmful to human body, the use of such antibacterial agent is recently avoided It is true.
섬유유연제는 세탁 후 섬유에 유연성을 부여하기 위한 마무리제로서, 통상 섬유에 대한 유연성 부여 효과와 함께 대전방지 효과를 제공한다.The fabric softening agent is a finishing agent for imparting flexibility to fibers after washing, and usually provides an effect of imparting flexibility to fibers as well as an antistatic effect.
종래에는 섬유유연제로서 디메틸 디알킬 암모늄 클로라이드 (dimethyl dialkyl ammonium chloride DDAC)가 널리 사용되었으나, 이후 아미도아민의 4급 암모늄염, 이미다졸린, 이미다졸린 에스터계의 섬유유연제를 거쳐, 현재는 지방산과 3급 아민으로부터 유도되는 에스터 화합물을 4급화하여 에스터쿼터 형태로 제조되는 양이온 계면활성제를 포함하는 섬유유연제가 전세계적으로 가장 많이 사용되고 있다. 그러나 상기 섬유 유연제의 제조시 사용되는 지방산이 고가이기 때문에 최근에는 원가 절감을 위해 고가의 지방산을 대체하여 식물성 오일로부터 섬유유연제를 제조하는 방법이 개발되고 있다.Conventionally, dimethyl dialkyl ammonium chloride (DDAC) has been widely used as a fabric softening agent. After that, it has been used as a fabric softener of quaternary ammonium salt, imidazoline and imidazoline ester of amidoamine, BACKGROUND OF THE INVENTION [0002] Fiber softeners including quaternary amine-derived ester compounds quaternized to produce an ester quaternary form and containing a cationic surfactant are the most widely used in the world. However, since the fatty acid used in the production of the fabric softener is expensive, recently, a method of manufacturing a fabric softener from plant oil by replacing expensive fatty acid has been developed in order to reduce the cost.
오일을 이용한 섬유유연제 제조방법으로 미국특허 제5,869,716호는 알칼리금속의 수소화붕소 또는 알칼리토금속의 수소화붕소 등의 촉매 존재 하에서 오일과 하이드록시 관능기를 가진 3급 아민을 반응시킨 후, 결과로 수득된 생성물을 4급화제와 반응시키는 단계를 포함하는 섬유유연제의 제조방법을 개시하고 있다. As a method for producing a fabric softener using oil, U.S. Patent No. 5,869,716 discloses a method of reacting an oil with a tertiary amine having a hydroxy functional group in the presence of a catalyst such as boron hydride of an alkali metal or boron hydride of an alkaline earth metal, With a quaternizing agent to produce a fabric softener.
또한 미국특허 제6,906,025호 및 제7,001,879호는 수소화붕소나트륨, 또는 수소화붕소나트륨과 수산화칼슘의 촉매 존재 하에서 트리글리세라이드 형태의 오일과 아민을 에스터 교환반응시켜 섬유유연제를 제조하는 방법을 개시하고 있다.Also, U.S. Patent Nos. 6,906,025 and 7,001,879 disclose a method for producing a fabric softener by ester-exchange reaction of an oil and an amine in the form of triglyceride in the presence of sodium borohydride or sodium borohydride and calcium hydroxide.
그러나 상기 방법들에서와 같이 오일로부터 직접 양이온 섬유유연제를 제조하는 방법은 미전환 트리글리세라이드 형태의 오일 함량이 높거나, 제조된 섬유유연제의 색상이 좋지 못한 문제가 있다.However, as in the above methods, the method of producing the cationic fiber softener directly from the oil has a problem that the oil content of the untranslated triglyceride is high or the color of the fabric softener is poor.
이에 대해 강알칼리 및 수소화붕소계 촉매를 사용하여 미전환 트리글리세라이드의 함량을 낮추고, 색상을 개선하기 위한 방법이 제안되었으나, 이 방법 역시 미반응 트리글리세라이드의 함량이 높고, 색상 및 향취가 좋지 못하는 문제점이 있다. On the other hand, a method for lowering the content of untranslated triglyceride and improving hue by using a strong alkali and boron hydride catalyst has been proposed. However, this method also has a problem that the content of unreacted triglyceride is high and the color and flavor are poor have.
본 발명은 상기와 같은 종래의 문제를 해결하기 위해 안출된 것으로, 황산나트륨 알킬 에터를 주재료로 사용하면서 교반을 통한 반응으로 욕중유연제를 사용하여, 구김 및 주름 방지 효과를 발휘하고 염반 방지에도 우수한 욕중유연제 제조방법 및 그 제조방법에 의한 욕중유연제를 제공하고자 한다.Disclosure of the Invention The present invention has been conceived to solve the above-mentioned conventional problems. It is an object of the present invention to provide a bath softener which exhibits a wrinkle and wrinkle preventing effect by using a bath softening agent by reaction with stirring while using sodium sulfate alkyl ether as a main material, And to provide a bath softening agent by the production method.
상기 목적을 달성하기 위해 본 발명은 황산나트륨 알킬 에터 10~30중량%, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터 1~5중량%, 에틸렌디아민 테트라초산디나트륨 0.1~0.5중량%, 에틸렌디아민 테트라초산테트라나트륨 0.1~0.5중량%, 소듐 벤조에이트 0.1~0.5중량% 및 총 함량이 100중량%가 되도록 정제수를 준비하는 준비단계; 상기 정제수 일부에 황산나트륨 알킬 에터, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터를 용해 및 혼합하는 1차 반응단계; 상기 1차 반응단계에서 형성된 혼합물에 에틸렌디아민 테트라초산디나트륨, 에틸렌디아민 테트라초산테트라나트륨 및 소듐 벤조에이트를 첨가하고 나머지 정제수를 첨가하여 용해 및 혼합하는 2차 반응단계; 상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계; 상기 여과된 혼합물을 숙성시키는 숙성단계를 포함하는 욕중유연제 제조방법을 제공한다. In order to accomplish the above object, the present invention provides a process for producing a polytetrafluoroethylene copolymer comprising 10-30 wt% sodium alkyl sulfate, 1-5 wt% polyoxyethylene-polyoxypropylene alkyl ether, 0.1-0.5 wt% disodium ethylenediaminetetraacetate, Preparing purified water so that the total amount of sodium is 0.1 to 0.5% by weight, sodium benzoate is 0.1 to 0.5% by weight and the total amount is 100% by weight; A first reaction step in which a sodium sulfate alkyl ether and a polyoxyethylene-polyoxypropylene alkyl ether are dissolved and mixed in a part of the purified water; A second reaction step in which disodium ethylenediaminetetraacetate, tetra sodium ethylenediamine tetraacetate and sodium benzoate are added to the mixture formed in the first reaction step and the remaining purified water is added to dissolve and mix; A filtration step of removing impurities from the mixture formed in the second reaction step; And an aging step of aging the filtered mixture.
또한, 본 발명은 상기 1차 반응단계 및 2차 반응단계는 15~40℃에서 250~750rpm의 교반속도로 60~180분 동안 교반하는 것을 특징으로 하는 욕중유연제 제조방법을 제공한다. In addition, the present invention provides a method for producing a bath softener, wherein the first reaction step and the second reaction step are carried out at a stirring speed of from 15 to 40 DEG C at a speed of from 250 to 750 rpm for from 60 to 180 minutes.
또한, 본 발명은 상기 여과는 150~250Mesh의 망 또는 체에서 정밀 여과하고, 상기 숙성은 12~36시간 동안 숙성하는 것을 특징으로 하는 욕중유연제 제조방법을 제공한다.Further, the present invention provides a method for fabricating a bath softener, wherein the filtration is microfiltration in a net or sieve of 150 to 250 Mesh, and the aging is aged for 12 to 36 hours.
또한, 본 발명은 상기 제조방법으로 제조되는 것을 특징으로 하는 욕중유연제를 제공한다.In addition, the present invention provides a bath softener which is produced by the above-mentioned production method.
본 발명은 천연섬유 또는 합성섬유 등 다양한 섬유의 구김을 방지하고 주름형성을 억제하는 효과가 있다.The present invention has the effect of preventing creasing of various fibers such as natural fibers or synthetic fibers and suppressing the formation of wrinkles.
또한, 본 발명은 욕중에서 사용할 수 있고, 세탁과정에서 세제와 같이 사용가능하여 유연제의 작업성을 높이는 효과가 있다.Further, the present invention can be used in a bath, and can be used in the same way as a detergent in the course of washing, thereby improving the workability of the softening agent.
또한, 본 발명은 욕중유연제가 처리된 섬유의 마모 발생을 방지하는 효과가 있다. Further, the present invention has an effect of preventing the occurrence of abrasion of the fiber treated with the bath softening agent.
도 1은 본 발명에 의한 욕중유연제 제조방법의 공정도이다.1 is a process diagram of a method for producing a bath softening agent according to the present invention.
이하 본 발명에 첨부된 도면을 참조하여 본 발명의 바람직한 일실시예를 상세히 설명하기로 한다. 우선, 도면들 중, 동일한 구성요소 또는 부품들은 가능한 동일한 참조부호를 나타내고 있음에 유의하여야 한다. 본 발명을 설명함에 있어, 관련된 공지기능 혹은 구성에 대한 구체적인 설명은 본 발명의 요지를 모호하지 않게 하기 위하여 생략한다.Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.
본 명세서에서 사용되는 정도의 용어 '약', '실질적으로' 등은 언급된 의미에 고유한 제조 및 물질 허용오차가 제시될 때 그 수치에서 또는 그 수치에 근접한 의미로 사용되고, 본 발명의 이해를 돕기 위해 정확하거나 절대적인 수치가 언급된 개시 내용을 비양심적인 침해자가 부당하게 이용하는 것을 방지하기 위해 사용된다.As used herein, the terms " about, " " substantially, " " etc. ", when used to refer to a manufacturing or material tolerance inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.
도 1은 본 발명에 의한 욕중유연제 제조방법의 공정도이다.1 is a process diagram of a method for producing a bath softening agent according to the present invention.
본 발명은 도 1에 나타난 바와 같이 준비단계, 1차 반응단계, 2차 반응단계, 여과단계, 숙성단계를 포함하여 제조되는 욕중유연제에 관한 것이다.The present invention relates to a bath softener prepared as shown in Fig. 1, comprising a preparation step, a first reaction step, a second reaction step, a filtration step and an aging step.
상기 준비단계는 1차 반응단계, 2차 반응단계를 원활히 진행할 수 있도록 사용되는 소재를 준비하는 단계로 황산나트륨 알킬 에터 10~30중량%, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터 1~5중량%, 에틸렌디아민 테트라초산디나트륨 0.1~0.5중량%, 에틸렌디아민 테트라초산테트라나트륨 0.1~0.5중량%, 소듐 벤조에이트 0.1~0.5중량% 및 총 함량이 100중량%가 되도록 정제수를 준비하는 단계이다.The preparation step may include preparing 10 to 30 wt% of sodium sulfate alkyl ether, 1 to 5 wt% of polyoxyethylene-polyoxypropylene alkyl ether, 0.1 to 0.5% by weight of disodium ethylenediaminetetraacetate, 0.1 to 0.5% by weight of ethylenediaminetetraacetate tetrasodium, 0.1 to 0.5% by weight of sodium benzoate, and 100% by weight of total amount.
상기 1차 반응단계는 정제수 일부에 황산나트륨 알킬 에터, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터를 용해 및 혼합하는 단계이다.The first reaction step is a step of dissolving and mixing sodium sulfate alkyl ether and polyoxyethylene-polyoxypropylene alkyl ether in a part of purified water.
상기 황산나트륨 알킬 에터는 주성분으로 균염 및 시와방지제로 작용한다.The sodium sulfate alkyl ether is a main component and functions as a salt solution and an anticorrosive agent.
상기 황산나트륨 알킬 에터는 음이온성 수지로 음이온 계면활성제로 작용하여 물에 녹으면 전리해 계면활성을 나타내는 부분이 음이온인 것을 특징으로 한다. The sodium sulfate alkyl ether is an anionic resin and acts as an anionic surfactant, and when it is dissolved in water, it is anion which is ionized to exhibit ionizing surface activity.
상기 황산나트륨 알킬 에터는 수용액상에서 세정, 습윤, 유화 등의 활성을 나타낼 수 있어 각종 세제로 많이 사용된다.The sodium sulfate alkyl ether can exhibit activities such as washing, wetting, and emulsifying in an aqueous solution, and is widely used as various detergents.
상기 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터는 보조성분으로 분산 및 유연제로 작용하여, 유연제 처리 대상의 구김 및 주름형성을 방지하고 부드러운 촉감을 형성할 수 있다.The polyoxyethylene-polyoxypropylene alkyl ether is dispersed as an auxiliary component and acts as a softening agent, so that creasing and wrinkling of the softener-treated object can be prevented and a soft touch can be formed.
상기 1차 반응단계는 각 성분의 변성을 막기 위해 15~40℃에서 250~750rpm의 교반속도로 60~180분간 교반하는 것이 바람직하며, 더욱 바람직하게는 20~30℃에서 400~600rpm의 교반속도로 100~140분간 교반하는 것이다.In order to prevent denaturation of each component, the first reaction step is preferably carried out at a stirring speed of from 250 to 750 rpm at a temperature of from 15 to 40 rpm for 60 to 180 minutes, more preferably at a stirring speed of from 400 to 600 rpm With stirring for 100 to 140 minutes.
상기 2차 반응단계는 1차 반응단계에서 형성된 혼합물에 에틸렌디아민 테트라초산디나트륨, 에틸렌디아민 테트라초산테트라나트륨 및 소듐 벤조에이트를 첨가하고 나머지 정제수를 첨가하여 용해 및 혼합하는 단계이다. In the second reaction step, disodium ethylenediaminetetraacetate, tetra sodium ethylenediamine tetraacetate and sodium benzoate are added to the mixture formed in the first reaction step, and the remaining purified water is added to dissolve and mix the mixture.
상기 에틸렌디아민 테트라초산디나트륨은 산성의 금속이온 봉쇄제로 작용하고, 상기 에틸렌디아민 테트라초산테트라나트륨은 알칼리성의 금속이온봉쇄제로 작용한다. 또한, 둘 다 금속이온 중에서도 철이온을 봉쇄하는 주된 기능을 가진다.The disodium ethylenediaminetetraacetate acts as an acidic sequestering agent, and the ethylenediaminetetraacetate tetrasodium acts as an alkaline sequestering agent. In addition, both of them have a main function of blocking iron ions among metal ions.
상기 금속이온 봉쇄제는 수용액 속에서 금속이온과 결합하여 가용성 킬레이트 착물을 형성하는 것으로, 수용액 중 염색시 수질에 혼입된 금속이온을 킬레이트화 시켜 금속의 분리 또는 경수를 연수화 하려는 등의 목적으로 사용된다.The metal ion sequestering agent binds to metal ions in an aqueous solution to form a soluble chelate complex. The metal ion sequestering agent is used for chelating metal ions incorporated in water during dyeing in an aqueous solution to separate metals or soften water do.
상기 금속이온봉쇄제는 욕중유연제에 혼입된 금속이온이 욕중유연제를 산패, 변질, 변색 등을 일으키는 것을 방지할 수 있다.The metal ion sequestrant can prevent the metal ions incorporated in the bath softening agent from causing spoilage, alteration, discoloration or the like of the bath softener.
상기 소듐 벤조에이트는 욕중유연제 내의 세균이 생육되는 것을 억제하여 보존성을 높이는 작용을 하는 방부제로 작용한다.The sodium benzoate acts as an antiseptic agent which acts to inhibit the growth of bacteria in the bath softener and to enhance preservability.
상기 2차 반응단계는 상기 1차 반응단계와 같이 각 성분의 변성을 막기 위해 15~40℃에서 250~750rpm의 교반속도로 60~180분간 교반하는 것이 바람직하며, 더욱 바람직하게는 20~30℃에서 400~600rpm의 교반속도로 80~100분간 교반하는 것이다.The second reaction step is preferably carried out at a stirring rate of 250 to 750 rpm at a temperature of 15 to 40 DEG C for 60 to 180 minutes to prevent denaturation of each component as in the first reaction step, more preferably 20 to 30 DEG C At a stirring speed of 400 to 600 rpm for 80 to 100 minutes.
상기 여과단계는 상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 단계로 150~250mesh의 필터를 사용하여 상기 1차, 2차 반응단계에서 생성될 수 있는 고형의 불순물을 제거한다.The filtration step is a step of removing impurities from the mixture formed in the second reaction step and removes solid impurities which may be generated in the first and second reaction steps using a filter of 150 to 250 mesh.
상기 숙성단계는 여과된 혼합물을 숙성시키는 단계로 밀폐된 공간에서 12~36시간 숙성시켜 제조되는 욕중유연제가 안정화되어 보존성을 높일 수 있다.The aging step is a step of aging the filtered mixture. The bath softening agent prepared by aging in a closed space for 12 to 36 hours can be stabilized to enhance the preservability.
또한 본 발명은 상기 방법에 의하여 제조된 욕중유연제도 포함한다.The present invention also includes a bath softener prepared by the above method.
상기의 제조된 욕중유연제는 안정성이 향상된 유연제를 제공하여 섬유 또는 원단의 염색가공, 후가공시 욕중에 포함되어 사용할 수 있으며, 세탁과정에서 세제와 같이 사용할 수 있을 것이다.The prepared bath softener may be used in the bath during dyeing or post-processing of fibers or fabrics by providing a softener having improved stability, and may be used together with a detergent in the washing process.
이하, 본 발명의 실시 예를 들어 상세히 설명한다. 단, 하기 실시 예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기 실시 예에 한정되는 것은 아니다.Hereinafter, embodiments of the present invention will be described in detail. However, the following examples are illustrative of the present invention, and the present invention is not limited to the following examples.
실시예Example
(1) 15~25℃에서 용해부(dissolve tank)에 정제수를(800kg)을 평량하여 넣고, 다음은 황산나트륨 알킬 에터(250kg), 폴리 옥시에틸렌-폴리옥시프로필렌 알킬 에터(50kg)을 용해부에 첨가한 후, 반응속도는 500RPM, 반응시간은 60분으로 설정하여 1차 반응단계를 실시한다.(1) Purified water (800 kg) was weighed into a dissolve tank at 15 to 25 ° C, followed by sodium sulfate alkyl ether (250 kg) and polyoxyethylene-polyoxypropylene alkyl ether (50 kg) After the addition, the reaction rate is set to 500 RPM, and the reaction time is set to 60 minutes to carry out the first reaction step.
(2) 15~25℃에서 정제수를(800kg)과 에틸렌디아민테트라초산디나트륨(5kg), 에틸렌디아민테트라초산테트라나트륨(5kg) 및 소듐벤조에이트(5kg)을 첨가 후, 반응속도는 500RPM, 반응시간은 60분으로 설정하여 2차 반응단계를 실시한다.(2) After adding purified water (800 kg), disodium ethylenediaminetetraacetate (5 kg), ethylenediaminetetraacetic acid tetrasodium (5 kg) and sodium benzoate (5 kg) at 15 to 25 ° C, the reaction rate was 500 RPM, The time is set to 60 minutes to carry out the second reaction step.
(3) 상기 2차 반응한 혼합물을 200Mesh의 망으로 정밀 여과시키고 24시간 동안 숙성단계를 거쳐 본 발명의 욕중유연제를 제조하였다.(3) The second-order reaction mixture was microfiltrated with a 200 mesh screen and aged for 24 hours to prepare a bath softener of the present invention.
상기 실시예에 의해 제조된 욕중유연제의 pH값은 8.60이며 당도값은 8.0이며, 성상(외관)은 연황색 투명 액상이다.The pH value of the bath softener prepared by the above example was 8.60, the sugar value was 8.0, and the appearance (appearance) was a pale yellow transparent liquid.
또한, 백금 도가니 내에 시료(욕중유연제) 10g을 넣고 150℃에서 30분간 가열한 후 냉각시켜 얻은 고형분은 8.0%이다.Further, 10 g of a sample (bath softening agent) was placed in a platinum crucible, and the solid content obtained by heating at 150 캜 for 30 minutes and cooling was 8.0%.
◈ 물성 평가◈ Property evaluation
(1) 방추도 평가(1) Spindle evaluation
본 발명의 욕중유연제를 3% o.w.f의 용액을 제조하고 폴리에스테르사로 제조된 원단(10g)을 용액에 침지, 교반하여 욕중유연제를 처리 및 건조하고, 욕중유연제를 처리 전, 후의 방추도를 평가하였다.A solution of the bath softening agent of the present invention in an amount of 3% owf was prepared, the fabric (10 g) made of polyester yarn was immersed in the solution and stirred to treat and dry the bath softener, and the degree of swelling before and after the treatment with the bath softener was evaluated .
상기 방추도는 KS K 0550:2011 B법(신장법)으로 시험하였다.The spindle was tested according to KS K 0550: 2011 B method (elongation method).
Oblique direction
Weft direction
표 1에서 나타난 바와 같이 본 발명의 욕중유연제를 처리한 경우 경사 및 위사방향에서 모두 표면과 표면의 방추도는 증가한 것을 알 수 있으며, 이면과 이면의 방추도는 저하된 것을 알 수 있다.As shown in Table 1, when the bath softening agent of the present invention was treated, it was found that the degree of skewness of the surface and the surface increased in both the warp and weft directions, and the degree of skewness of the back surface and the back surface decreased.
(2) 유연성 및 착용감 관능 평가(2) Flexibility and fit sensory evaluation
본 발명의 욕중유연제를 3% o.w.f의 용액을 제조하고 면/PET가 중량비 7/3인 혼방사로 제조된 티셔츠를 상기 용액에 침지하여 욕중유연제를 처리 및 건조하고, 욕중유연제를 처리 전, 후의 유연성을 평가하였다.The bath softener of the present invention was prepared by preparing a solution of 3% owf, and a t-shirt made of a cotton / PET blend with a weight ratio of 7/3 was immersed in the solution to treat and dry the bath softener, .
1. 평가방법 : 욕중유연제로 처리 전, 후의 티셔츠를 고정된 패널에게 목에 각각 착용시키고, 1시간 동안 걷기를 실시한 후에 유연성 및 착용감을 관능평가하였다.1. Evaluation method: The t-shirts before and after the treatment with the bath softener were worn on a fixed panel to the neck, respectively, and after walking for 1 hour, the flexibility and comfortability were evaluated.
2. 고정된 패널 : 일반인 10명2. Fixed panel: 10 people in general
3. 채점방법 : 유연성 효과는 매우좋다 5점, 좋다 4점, 보통이다 3점, 나쁘다 2점 매우나쁘다 1점으로 채점하여 평균을 내었으며 착용감은 10점 만점으로 채점하여 걷기 전과 후를 평가하고, 평균을 내어, 표 2에 나타내었다.3. Scoring method: Flexibility effect is very good 5 points, good 4 points, average 3 points, worse 2 points Very bad 1 point score and average score. Wear feeling is evaluated as 10 points, before and after walking Are averaged, and are shown in Table 2.
flexibility
표 1에 나타난 바와 같이 본 발명의 욕중유연제를 처리 후의 유연성 평가는 처리 전의 유연성 평가보다 높게 평가된 것으로 본 발명의 욕중유연제는 섬유의 유연성을 높이는 작용을 하는 것을 알 수 있다.As shown in Table 1, the flexibility evaluation after treatment of the bath softening agent of the present invention was evaluated to be higher than the flexibility evaluation before treatment, and it can be seen that the bath softening agent of the present invention enhances the flexibility of the fiber.
또한, 걷기를 1시간 시킨 후에 착용감에서는 욕중유연제로 처리된 티셔츠는 걷기 전과 후가 착용감에서 큰 차이가 없이 높이 평가되었으나, 실리콘계 욕중유연제로 처리되기 전인 티셔츠는 걷기 전과 후가 착용감에서 차이가 크고, 욕중유연제 처리 후 보다 착용감이 떨어지는 것을 알 수 있다.Also, after 1 hour of walking, the t - shirts treated with the bath softener showed a high degree of comfort before and after walking, but the t - shirts before the treatment with the silicone based bath softener showed a large difference in wearing comfort before and after walking, It can be seen that the feeling of comfort is lower after treatment with the bath softener.
욕중유연제를 처리함으로써 원단 자체의 유연성도 향상시키고, 이로 인해 착용시 쾌적함을 제공하며 운동 후에도 착용감이 유지되는 것을 확인할 수 있다.By treating the bath softener, the flexibility of the fabric itself is also improved, thereby providing comfort during wearing and maintaining the fit after exercise.
이상에서 설명한 본 발명은 전술한 실시예에 의해 한정되는 것이 아니고, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환, 변형 및 변경이 가능함은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에게 있어서 명백할 것이다.While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be clear to those who are.
Claims (4)
상기 정제수 일부에 황산나트륨 알킬 에터, 폴리옥시에틸렌-폴리옥시프로필렌 알킬 에터를 첨가하고 15~45℃에서 250~750rpm의 교반속도로 60~180분간 교반하면서 용해 및 혼합하는 1차 반응단계;
상기 1차 반응단계에서 형성된 혼합물에 에틸렌디아민 테트라초산디나트륨, 에틸렌디아민 테트라초산테트라나트륨 및 소듐 벤조에이트를 첨가하고 나머지 정제수를 첨가하여 15~45℃에서 250~750rpm의 교반속도로 60~180분간 교반하면서 용해 및 혼합하는 2차 반응단계;
상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계;
상기 여과된 혼합물을 밀폐된 공간에서 12~36시간 숙성시키는 숙성단계를 포함하는 욕중유연제의 제조방법.
10 to 30% by weight of sodium sulfate alkyl ether, 1 to 5% by weight of polyoxyethylene-polyoxypropylene alkyl ether, 0.1 to 0.5% by weight of disodium ethylenediaminetetraacetate, 0.1 to 0.5% by weight of tetrasodium ethylenediamine tetraacetate, Preparing 0.1 to 0.5% by weight of purified water and a total amount of 100% by weight;
A first reaction step of adding sodium sulfate alkyl ether and polyoxyethylene-polyoxypropylene alkyl ether to a part of the purified water and dissolving and mixing at 15 to 45 ° C with stirring at a stirring speed of 250 to 750 rpm for 60 to 180 minutes;
Disodium ethylenediaminetetraacetate, tetra sodium ethylenediaminetetraacetate, and sodium benzoate were added to the mixture formed in the first reaction step, the remaining purified water was added, and the mixture was stirred at a temperature of 15 to 45 DEG C at a stirring rate of 250 to 750 rpm for 60 to 180 minutes A second reaction step of dissolving and mixing with stirring;
A filtration step of removing impurities from the mixture formed in the second reaction step;
And aging the filtered mixture in an enclosed space for 12 to 36 hours.
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WO2012136427A1 (en) | 2011-04-04 | 2012-10-11 | Unilever Plc | Method of laundering fabric |
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WO2012136427A1 (en) | 2011-04-04 | 2012-10-11 | Unilever Plc | Method of laundering fabric |
WO2015164515A1 (en) | 2014-04-22 | 2015-10-29 | The Sun Products Corporation | Unit dose detergent compositions |
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