KR101886399B1 - Textile softener of silicone type and it's manufacturing method thereof - Google Patents
Textile softener of silicone type and it's manufacturing method thereof Download PDFInfo
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- KR101886399B1 KR101886399B1 KR1020160105094A KR20160105094A KR101886399B1 KR 101886399 B1 KR101886399 B1 KR 101886399B1 KR 1020160105094 A KR1020160105094 A KR 1020160105094A KR 20160105094 A KR20160105094 A KR 20160105094A KR 101886399 B1 KR101886399 B1 KR 101886399B1
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 229920001296 polysiloxane Polymers 0.000 title claims description 34
- 239000004753 textile Substances 0.000 title description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000008213 purified water Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 11
- 235000011187 glycerol Nutrition 0.000 claims abstract description 11
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 11
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 11
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 11
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical class [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 239000002979 fabric softener Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 239000004744 fabric Substances 0.000 description 16
- 239000004902 Softening Agent Substances 0.000 description 11
- 239000000835 fiber Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000012805 post-processing Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 125000003277 amino group Chemical group 0.000 description 3
- 229920013822 aminosilicone Polymers 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- -1 quaternary ammonium salt compound Chemical class 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004925 denaturation Methods 0.000 description 2
- 230000036425 denaturation Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000003676 hair preparation Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013077 scoring method Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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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
-
- 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
- C11D3/162—Organic compounds containing Si
-
- 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
- C11D3/2003—Alcohols; Phenols
-
- 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 변성 아미노 실리콘 10~45중량%, 글리세린 1~10 중량%, 소디움 벤조에이트 0.1~1중량%, 구연산 0.05~1중량%, 및 총 함량이 100중량%가 되도록 정제수를 준비하는 준비단계; 상기 정제수에 변성 아미노 실리콘, 글리세린을 첨가하여 교반하면서 용해 및 혼합하는 1차 반응단계; 상기 1차 반응단계에서 증발된 정제수를 보충하고 소디움 벤조에이트과 구연산을 첨가하여 교반하면서 용해 및 혼합하는 2차 반응단계; 상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계; 및, 여과된 혼합물을 숙성시키는 숙성단계를 포함하는 것을 특징으로 하는 실리콘계 섬유유연제 및 그의 제조방법에 관한 것이다.The present invention relates to a process for preparing purified water so that the total amount of purified water is 10 to 45 wt% of modified amino silicon, 1 to 10 wt% of glycerin, 0.1 to 1 wt% of sodium benzoate, 0.05 to 1 wt% of citric acid, ; A first reaction step in which modified amino silicon and glycerin are added to the purified water and dissolved and mixed while stirring; A second reaction step of replenishing the purified water evaporated in the first reaction step and adding sodium benzoate and citric acid to dissolve and mix while stirring; A filtration step of removing impurities from the mixture formed in the second reaction step; And an aging step of aging the filtered mixture, and a process for producing the same.
Description
본 발명은 실리콘계 섬유유연제 및 그의 제조방법에 관한 것으로 신규한 제조방법을 통해 섬유원단의 촉감 및 유연성을 향상시킬 수 있는 실리콘계 섬유유연제 및 그의 제조방법에 관한 것이다.TECHNICAL FIELD The present invention relates to a silicone-based fabric softener and a method for producing the same, and relates to a silicone-based fabric softener capable of improving tactility and flexibility of a fiber fabric through a novel manufacturing method and a manufacturing method thereof.
일반적으로 천연섬유, 합성섬유 등으로 형성되는 섬유 제품은 염색공정과 다양한 후가공 공정을 거치는데, 후가공 공정 중 하나로 섬유의 촉감을 개선하고 유연성을 향상시키기 위해 섬유유연제를 사용하여 섬유제품에 착용감을 부여하는 공정이 실시되고 있다.In general, textile products made of natural fibers and synthetic fibers are subjected to dyeing process and various post-processing processes. One of the post-processing processes is to give a feeling of fit to the textile products by using a fabric softener to improve the feeling of the fiber and improve the flexibility. Are carried out.
상기 섬유유연제와 같은 섬유 가공제는 섬유산업의 성장과 함께 발전해왔으나, 기초화학 및 응용화학의 핵심기술과 인프라가 극히 부족하여 90년대 초반까지 일본을 비롯한 미국과 유럽 등지에서 원료를 들여와 혼합하는 기초적 조제 단계를 벗어나지 못하다가 90년 중반 이후, 비로소 기초적 합성과 고분자 화합물로 이루어진 조제를 생산하고 있다.Textile processing agents such as fabric softeners have been developed along with the growth of the textile industry. However, the core technologies and infrastructure of basic and applied chemistry have been extremely inadequate, so that until the early 1990s, basic raw materials were imported from Japan and other countries, It does not escape from the preparation stage, but after the middle of 1990, it produces basic preparations and preparations consisting of polymer compounds.
대한민국 등록특허 제0259423호는 투명 액상 섬유유연제 조성물에 관한 것으로 양이온성 유연성분으로서 자기분산성이 우수한 디알킬알카놀 4급 암모늄염 화합물과 500 내지 3000이하의 폴리프로폭시 4급 암모늄염 화합물 중에서 선택된 하나 이상을 3 내지 45 중량% 포함하여 구성되어 유연성 및 정전기 방지성의 기능을 섬유원단에 부여하는 기능을 가지며, 대한민국 등록특허 제0777010호는 내알칼리성이 우수한 자기유화형 아미노오일 섬유유연제에 관한 것으로 알킬렌 변성 폴리실록산과 폴리알킬렌옥사이드의 교대 단위로 구성된 블록 공중합체로서 가교 가능성이 적어 안정적이면서도 간단한 방법으로 제조될 수 있고, 내알칼리성, 유연성 및 재염성이 우수한 섬유유연제에 관한 것이다.Korean Patent Registration No. 0259423 relates to a transparent liquid fabric softener composition which comprises a cationic softening component comprising at least one member selected from a dialkyl alkanol quaternary ammonium salt compound having excellent self dispersibility and a polypropoxy quaternary ammonium salt compound having a molecular weight of 500 to 3000 or less , And 3 to 45% by weight, and has the function of imparting the function of flexibility and antistatic property to the fiber fabric. Korea Patent No. 0777010 relates to a self emulsifying amino oil fabric softener excellent in alkali resistance, A block copolymer composed of alternating units of polysiloxane and polyalkylene oxide, which is less likely to be crosslinked and can be produced in a stable and simple manner, and is excellent in alkali resistance, flexibility and remineralization.
상기와 같이 국내 기업에서 개발된 섬유유연제는 유연성 기능에 초점을 두어 개발된 것으로 섬유원단에 필요한 기능을 부여하기 위해서는 추가적인 후가공이 필요하여 생산성 효율이 높지 않은 문제점이 있다.As described above, the fabric softener developed in a domestic company has been developed with a focus on the flexibility function, and in order to give the necessary function to the fabric, additional post-processing is required, and the productivity efficiency is not high.
이와 같이 섬유용 계면활성제에서 조제의 발전 없이 섬유산업의 발전은 기대할 수 없으며, 중국, 베트남 등 섬유후발개도국과의 경쟁에서 우위를 점하고, 섬유선진국 대열에 진입하기 위해서는 섬유제품의 고부가가치에 절대적으로 기여하는 염료, 계면활성제, 조제 분야의 연구가 필수적이다.In this way, the development of the textile industry can not be expected without the development of preparations for textile surfactants. In order to enter the ranks of textile advanced countries, Researches in the fields of dyes, surfactants,
또한, 상기 섬유유연제는 다양한 성분들이 조합되는 것으로 장시간 보관시에는 화합물이 서로 화학반응을 통해 물성의 변화가 발생되는 안정성이 떨어지는 문제가 있으며, 최근에는 기능 면에서도 고효율의 제품수준이 요구되고 있는 상황이다.In addition, the fabric softener has a problem in that stability is low due to a change in physical properties through chemical reaction between the compounds when stored for a long period of time. In recent years, there has been a demand for a high- to be.
본 발명은 상기와 같은 종래기술의 문제점을 해결하기 위해 발명된 것으로 변성 아미노 실리콘을 주재료로 사용하면서 교반을 통한 반응으로 안정성이 향상된 실리콘계 섬유유연제 제조방법을 제공하는 것을 목적으로 한다.Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made in an effort to solve the problems of the prior art as described above, and it is an object of the present invention to provide a method of manufacturing a silicone-based fabric softener having improved stability by using a modified amino silicone as a main material while stirring.
또한, 상기의 제조방법으로 제조되는 실리콘계 섬유유연제를 제공하는 것을 목적으로 한다.It is another object of the present invention to provide a silicone-based fabric softening agent produced by the above-mentioned production method.
본 발명은 변성 아미노 실리콘 10~45중량%, 글리세린 1~10 중량%, 소디움 벤조에이트 0.1~1중량%, 구연산 0.05~1중량%, 및 총 함량이 100중량%가 되도록 정제수를 준비하는 준비단계; 상기 정제수에 변성 아미노 실리콘, 글리세린을 첨가하여 교반하면서 용해 및 혼합하는 1차 반응단계; 상기 1차 반응단계에서 증발된 정제수를 보충하고 소디움 벤조에이트과 구연산을 첨가하여 교반하면서 용해 및 혼합하는 2차 반응단계; 상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계; 및, 여과된 혼합물을 숙성시키는 숙성단계를 포함하는 것을 특징으로 하는 실리콘계 섬유유연제 제조방법을 제공한다.The present invention relates to a process for preparing purified water so that the total amount of purified water is 10 to 45 wt% of modified amino silicon, 1 to 10 wt% of glycerin, 0.1 to 1 wt% of sodium benzoate, 0.05 to 1 wt% of citric acid, ; A first reaction step in which modified amino silicon and glycerin are added to the purified water and dissolved and mixed while stirring; A second reaction step of replenishing the purified water evaporated in the first reaction step and adding sodium benzoate and citric acid to dissolve and mix while stirring; A filtration step of removing impurities from the mixture formed in the second reaction step; And an aging step of aging the filtered mixture. The present invention also provides a method for producing a silicone-based fabric softening agent.
또한, 상기 1차 반응단계 및 2차 반응단계는 15~30℃에서 250~750rpm의 교반속도로 60~180분간 교반하는 것을 특징으로 하는 실리콘계 섬유유연제 제조방법을 제공한다.Also, the first reaction step and the second reaction step may be carried out at a stirring speed of from 250 to 750 rpm at a temperature of from 15 to 30 DEG C for 60 to 180 minutes.
또한, 상기 숙성단계는 밀폐된 공간에서 12~36시간 숙성시키는 것을 특징으로 하는 실리콘계 섬유유연제 제조방법을 제공한다.In addition, the present invention provides a method for manufacturing a silicone-based fabric softener, wherein the aging is aged in a closed space for 12 to 36 hours.
또한, 상기의 제조방법으로 제조되는 것을 특징으로 하는 실리콘계 섬유유연제를 제공한다.Also, there is provided a silicone-based fabric softener which is produced by the above-mentioned production method.
본 발명은 상기와 같이 종래기술의 문제점을 해결하기 위해 발명된 것으로 변성 아미노 실리콘을 주재료로 사용하면서 교반을 통한 반응으로 안정성이 향상된 실리콘계 섬유유연제을 제조할 수 있는 효과가 있다. The present invention has been made to solve the problems of the prior art as described above, and it is possible to produce a silicone-based fabric softener having improved stability by using a modified amino silicone as a main material while stirring.
또한, 본 발명의 실리콘계 섬유유연제는 섬유 또는 원단의 염색가공, 후가공 욕중에 사용할 수 있고, 세탁과정에서 세제와 같이 사용할 수도 있어 사용상 이용이 편리하여 작업성을 높이는 효과가 있다.In addition, the silicone-based fabric softening agent of the present invention can be used in dyeing or post-processing of fibers or fabrics, and can be used in combination with a detergent in the course of washing.
도 1은 본 발명에 따른 실리콘계 섬유유연제 제조방법의 공정도이다.1 is a process diagram of a method for producing a silicone-based fabric softener 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 따른 실리콘계 섬유유연제 제조방법의 공정도이다.1 is a process diagram of a method for producing a silicone-based fabric softener according to the present invention.
본 발명은 도 1에 나타난 바와 같이 준비단계, 1차 반응단계, 2차 반응단계, 여과단계, 숙성단계를 포함하여 제조되는 실리콘계 섬유유연제에 관한 것이다.The present invention relates to a silicone-based fabric 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 변성 아미노 실리콘 10~45중량%, 글리세린 1~10 중량%, 소디움 벤조에이트 0.1~1중량%, 구연산 0.05~1중량%, 및 총 함량이 100중량%가 되도록 정제수를 준비하는 단계이다.The preparation step is a step of preparing a material to be used so that the first reaction step and the second reaction step can be progressed smoothly. The preparation step comprises 10 to 45 wt% of modified amino silicon, 1 to 10 wt% of glycerin, 0.1 to 1 wt% of sodium benzoate, 0.05 to 1% by weight citric acid, and a total content of 100% by weight.
상기 1차 반응단계는 정제수에 변성 아미노 실리콘, 글리세린을 첨가하여 교반하면서 용해 및 혼합하는 단계이다.The first reaction step is a step of adding denatured amino silicone and glycerin to purified water and dissolving and mixing with stirring.
상기 아미노변성 실리콘은 분자 중에 아미노기를 함유하기 때문에 음전하를 띠는 섬유에 양전하의 아미노기가 부착되게 하여 오랫동안 부드러운 지속성을 부여하는 작용으로 섬유의 통풍성, 유연성, 농염효과를 부여하는 특성이 있어 섬유유연제 또는 두발용 화장품에 많이 사용되고 있다.Since the amino-modified silicone contains an amino group in the molecule, the amino group of positive charge is adhered to the negatively charged fiber and gives the soft sustenance for a long time. Thus, the amino-modified silicone imparts the permeability, flexibility, It is widely used in hair cosmetics.
본 발명에서 사용되는 아미노변성 실리콘의 점도가 100 cP 미만이거나 80,000cP를 초과하면 공정상의 문제가 발생될 수 있으므로 아미노변성 실리콘의 점도는 100~80,000 cP인 것이 바람직하며, 더욱 바람직하게는 500~2,000cP이다.When the viscosity of the amino-modified silicone used in the present invention is less than 100 cP or more than 80,000 cP, a problem may arise in the process. Therefore, the viscosity of the amino-modified silicone is preferably 100 to 80,000 cP, more preferably 500 to 2,000 cP.
또한, 아미노변성 실리콘의 아민기 함량이 0.01중량% 미만이면 섬유에 유연성 부여효과가 저하될 수 있으며, 1.5중량%를 초과하면 섬유유연제가 갈변화될 수 있으므로 아미노변성 실리콘의 아민기 함량은 아미노변성 실리콘 총 중량 기준으로 0.01~1.5중량%인 것이 바람직할 것이다.If the amine group content of the amino-modified silicone is less than 0.01% by weight, the effect of imparting flexibility to the fiber may be deteriorated. If the content of the amine softener exceeds 1.5% by weight, Preferably, it is 0.01 to 1.5 wt% based on the total weight of silicon.
상기 글리세린은 유지 성분으로 공기중의 수분을 흡수하여 섬유에 보습력을 높이는 작용을 한다.The glycerin absorbs moisture in the air as a retaining component and acts to increase the moisture resistance of the fibers.
상기 1차 반응단계는 각 성분의 변성을 막기 위해 15~30℃에서 250~750rpm의 교반속도로 60~180분간 교반하는 것이 바람직하며, 더욱 바람직하게는 15~25℃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 rate of 250 to 750 rpm at 15 to 30 ° C for 60 to 180 minutes, more preferably at a stirring rate of 400 to 600 rpm at 15 to 25 ° C With stirring for 100 to 140 minutes.
상기 2차 반응단계는 1차 반응단계에서 증발된 정제수를 보충하고 소디움 벤조에이트과 구연산을 첨가하여 교반하면서 용해 및 혼합하는 단계이다.In the second reaction step, purified water evaporated in the first reaction step is supplemented, sodium benzoate and citric acid are added and dissolved and mixed while stirring.
상기 소디움 벤조에이트는 섬유유연제 내의 세균이 생육되는 것을 억제하여 보존성을 높이는 작용을 한다.The sodium benzoate inhibits the growth of bacteria in the fabric softener and enhances preservability.
상기 구연산은 섬유유연제의 pH를 조절하는 작용으로 섬유유연제의 pH가 약5.0~6.0인 약산성을 가지도록 사용량을 조절하여야 할 것이다.The amount of citric acid should be controlled so that the pH of the fabric softening agent is adjusted to have a pH of about 5.0 to 6.0.
상기 2차 반응단계는 상기 1차 반응단계와 같이 각 성분의 변성을 막기 위해 15~30℃에서 250~750rpm의 교반속도로 60~180분간 교반하는 것이 바람직하며, 더욱 바람직하게는 15~25℃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 30 DEG C for 60 to 180 minutes to prevent denaturation of each component as in the first reaction step, At a stirring speed of 400 to 600 rpm for 80 to 100 minutes.
상기 여과단계는 상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 단계로 150~300mesh의 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 300 mesh.
상기 숙성단계는 여과된 혼합물을 숙성시키는 단계로 밀폐된 공간에서 12~36간 숙성시켜 제조되는 실리콘계 섬유유연제가 안정화되어 보존성을 높일 수 있다.The aging step is a step of aging the filtered mixture. The silicone-based fabric softening agent prepared by aging 12 to 36 days in an enclosed space is stabilized, and the preservability can be improved.
상기와 같이 제조되는 본 발명에 따른 실리콘계 섬유유연제는 섬유 또는 원단의 염색가공, 후가공 욕중에 포함되어 사용할 수 있으며, 세탁과정에서 세제와 같이 사용할 수 있을 것이다.The silicone-based fabric softener according to the present invention may be used in dyeing or post-processing of fibers or fabrics, and may be used as a detergent in the course of washing.
이하 본 발명에 따른 실리콘계 섬유유연제를 제조하기 위한 방법의 실시예를 나타내지만, 본 발명이 실시예로 한정되는 것은 아니다.Examples of the method for producing the silicone-based fabric softening agent according to the present invention are shown below, but the present invention is not limited to the examples.
실시예Example
실리콘계 섬유유연제의 재료인 변성 아미노 실리콘(점도 1,200~1,400cP, 아민함량 0.8~0.95중량%), 글리세린, 소디움 벤조에이트, 구연산을 준비한 후, 15~20℃에서 용해부(Dissolve Tank)에 정제수(1100kg)를 넣고 변성 아미노 실리콘(800kg)과 글리세린(100kg)을 첨가한 후, 500RPM과 2시간(hr)동안 교반시켜 1차 반응단계을 실시하였다.(Viscosity: 1,200 to 1,400 cP, amine content: 0.8 to 0.95% by weight), glycerin, sodium benzoate and citric acid, which are the materials of the silicone-based fabric softening agent, are prepared and then dissolved in a dissolving tank (800 kg) and glycerin (100 kg) were added, and the mixture was stirred at 500 RPM for 2 hours (hr) to carry out the first reaction step.
상기 1차 반응 단계 후에 소디움 벤조에이트(2kg)과 구연산(2kg)를 용해부에 첨가한 후 총 중량이 2000kg가 되도록 정제수를 보충한 후, 15~20℃에서 500RPM과 1.5시간(hr)동안 교반시켜 2차 반응단계를 실시하였다.After the first reaction step, sodium benzoate (2 kg) and citric acid (2 kg) were added to the dissolution part, and purified water was added thereto so that the total weight became 2000 kg. Then, the mixture was stirred at 15 to 20 ° C and 500 RPM for 1.5 hours Followed by a second reaction step.
상기 2차 반응단계 후에 200Mesh 필터를 사용하여 여과단계를 실시하고 24시간 숙성시키는 숙성단계를 통해 본 발명의 실리콘계 섬유유연제를 제조하였다.After the second reaction step, the silicone-based fabric softener of the present invention was prepared through a filtration step using a 200 Mesh filter and aging for aging for 24 hours.
제조된 실리콘계 섬유유연제의 pH는 5.35이며, 연청색 반투명액상으로 제조되었다.The pH of the prepared silicone-based fabric softener was 5.35, and it was prepared as a light blue translucent liquid.
◈ 물성 평가◈ Property evaluation
(1) 방추도 평가(1) Spindle evaluation
본 발명의 실리콘계 섬유유연제를 3% o.w.f의 용액을 제조하고 폴리에스테르사로 제조된 원단(10g)을 용액에 침지, 교반하여 실리콘계 섬유유연제 처리 및 건조하고, 섬유유연제 처리 전 후의 방추도를 평가하였다.A silicone-based fabric softening agent of the present invention was prepared by preparing a solution of 3% o.w.f, and the fabric (10 g) made of polyester yarn was immersed in the solution and stirred to treat and soften the silicone-based fabric softener.
상기 방추도는 KS K 0550:2011 B법(신장법)으로 시험하였다.The spindle was tested according to KS K 0550: 2011 B method (elongation method).
표 1에서 나타난 바와 같이 본 발명의 실리콘계 섬유유연제로 처리된 경우 경사 및 위사방향 모두 표면과 표면의 방추도는 증가한 것을 알 수 있으며, 이면과 이면의 방추도는 저하된 것을 알 수 있다.As shown in Table 1, when the silicone-based fabric softener of the present invention was treated with the softening agent of the present invention, it was found that the degree of wrinkling of the surface and the surface increased in both the warp and weft directions, and the degree of wrinkling of the back surface and the back surface was decreased.
(2) 유연성 및 착용감 관능 평가(2) Flexibility and fit sensory evaluation
본 발명의 실리콘계 섬유유연제를 3% o.w.f의 용액을 제조하고 면/PET가 중량비 7/3인 혼방사로 제조된 티셔츠를 상기 용액에 침지하여 실리콘계 섬유유연제 처리 및 건조하고, 섬유유연제 처리 전, 후의 유연성을 평가하였다.A silicone-based fabric softening agent 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 silicone-based fabric softener, .
1. 평가방법 : 섬유유연제로 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 treatment with a fabric softener were worn on a fixed panel to the neck, respectively, and walked for 1 hour.
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 The results are shown in Table 2.
flexibility
표 1에 나타난 바와 같이 본 발명의 실리콘계 섬유유연제를 처리 후의 유연성 평가는 처리 전의 유연성 평가보다 높게 평가된 것으로 본 발명의 섬유유연제는 섬유의 유연성을 높이는 작용을 하는 것을 알 수 있다.As shown in Table 1, the evaluation of flexibility after the treatment of the silicone-based fabric softener of the present invention was evaluated to be higher than the evaluation of flexibility before the treatment, and it can be seen that the fabric softener of the present invention has an effect of improving the flexibility of the fiber.
또한, 걷기를 1시간 시킨 후에 착용감에서는 실리콘계 섬유유연제로 처리된 티셔츠는 걷기 전과 후가 착용감에서 큰 차이가 없이 높이 평가되었으나, 실리콘계 섬유유연제로 처리되기 전인 티셔츠는 걷기 전과 후가 착용감에서 차이가 크고 섬유유연제 처리 후의 보다 착용감이 떨어지는 것을 알 수 있다.Also, after 1 hour of walking, the t-shirts treated with silicone-based fabric softener showed a high degree of comfort before and after walking, but before t-shirts treated with silicone-based fabric softener, It can be seen that the wearing feeling after the treatment with the fabric softening agent is lowered.
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 obvious to the person.
Claims (4)
상기 정제수에 변성 아미노 실리콘, 글리세린을 첨가하여 15~25℃에서 400~600rpm의 교반속도로 60~180분간 교반하면서 용해 및 혼합하는 1차 반응단계;
상기 1차 반응단계에서 증발된 정제수를 보충하고 소디움 벤조에이트과 구연산을 첨가하여 15~25℃에서 400~600rpm의 교반속도로 60~180분간 교반하면서 용해 및 혼합하는 2차 반응단계;
상기 2차 반응단계에서 형성된 혼합물에서 불순물을 제거하는 여과단계;
여과된 혼합물을 밀폐된 공간에서 12~36시간 숙성시키는 숙성단계를 포함하는 것을 특징으로 하는 실리콘계 섬유유연제 제조방법.
Preparing purified water so that the total amount of purified water is 10 to 45% by weight of modified amino silicon, 1 to 10% by weight of glycerin, 0.1 to 1% by weight of sodium benzoate, 0.05 to 1% by weight of citric acid, and a total content of 100% by weight.
A first reaction step of adding the modified amino silicon and glycerin to the purified water and dissolving and mixing the mixture at a stirring speed of from 15 to 25 ° C at a stirring speed of from 400 to 600 rpm for 60 to 180 minutes;
A second reaction step in which purified water evaporated in the first reaction step is supplemented and sodium benzoate and citric acid are added and dissolved and mixed at a stirring rate of 400 to 600 rpm at 15 to 25 ° C with stirring for 60 to 180 minutes;
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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| KR102434313B1 (en) | 2022-01-13 | 2022-08-18 | 강인숙 | Fabric softener of silicone for having improved stability of high temperature-alkali |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101423649B1 (en) | 2013-04-05 | 2014-08-01 | (주)시그마소재 | Textile softener base on self-emulsified type silicone oil |
| KR101502101B1 (en) | 2014-03-24 | 2015-03-12 | 주식회사 스노젠 | Composition having silicone based elasticity finishing agent for rubbing cloth |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2387883B2 (en) * | 2002-08-12 | 2017-03-22 | Lonza Inc. | Antimicrobial compositions comprising sodium benzoate |
| WO2004061197A1 (en) * | 2002-12-27 | 2004-07-22 | Lion Corporation | Liquid softener composition |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101423649B1 (en) | 2013-04-05 | 2014-08-01 | (주)시그마소재 | Textile softener base on self-emulsified type silicone oil |
| KR101502101B1 (en) | 2014-03-24 | 2015-03-12 | 주식회사 스노젠 | Composition having silicone based elasticity finishing agent for rubbing cloth |
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