보고서 정보
주관연구기관 |
충남대학교 Chungnam National University |
연구책임자 |
손영아
|
참여연구자 |
란가라쥬 사티쉬 쿠마르
,
라말린감 마니바난
,
메르구 나빈
,
김창겸
,
오우람
,
김익진
,
정재명
,
김명진
,
김창일
,
김지연
,
성상헌
,
신희정
|
보고서유형 | 1단계보고서 |
발행국가 | 대한민국 |
언어 |
한국어
|
발행년월 | 2017-11 |
과제시작연도 |
2016 |
주관부처 |
과학기술정보통신부 Ministry of Science and ICT |
등록번호 |
TRKO201800002920 |
과제고유번호 |
1711042947 |
사업명 |
STEAM연구 |
DB 구축일자 |
2018-04-14
|
키워드 |
광학적 고감도.스케일 업.마이크로캡슐레이션.가변패턴.군수용 섬유제품.Optical high sensitivity.Scale up.Micro-capsulated technology.Changeable pattern.military textiles.
|
DOI |
https://doi.org/10.23000/TRKO201800002920 |
초록
▼
■ 신규 감온색소재료의 설계, 합성 및 변색특성 개발
- Pariser-Parr-Pople MO, DMol3 계산을 이용한 신규 감온색소분자의 구조설계
- Leuco dye를 기반으로 한 chromophore의 골격을 이용하여 다양한 신규 감온색 소재료를 디자인, 합성하여 합성물질 분석 및 광학적 특성분석을 진행함.
- 광학적 고감도를 가진 Fluoran계 Self-Thermochromic, 신규 Betain 감온볂색 색소 합성.
■ 신규 감온색소재료의 Scale up 및 상용화 formulation 개발
■ 신규 감온색소재료의 설계, 합성 및 변색특성 개발
- Pariser-Parr-Pople MO, DMol3 계산을 이용한 신규 감온색소분자의 구조설계
- Leuco dye를 기반으로 한 chromophore의 골격을 이용하여 다양한 신규 감온색 소재료를 디자인, 합성하여 합성물질 분석 및 광학적 특성분석을 진행함.
- 광학적 고감도를 가진 Fluoran계 Self-Thermochromic, 신규 Betain 감온볂색 색소 합성.
■ 신규 감온색소재료의 Scale up 및 상용화 formulation 개발
- Lactone계/Amionfluoran계, BDF계, 신규 구조의 CVL 감온색소 합성 및 물성 평가
- 구조적으로 빛에 취약한 열변색 색소의 섬유 적용 시 변·퇴색을 최소화하기 위한 목적으로 내구성 증진제를 합성(Benzophenone류, Triazole류, Triazine류)
- 1~3년도 신규 개발염료 4종에 대한 Lab scale up(500g)
■ 감온색소를 담지하는 마이크로캡슐레이션 기술개발
- 비멜라민계 Styrene 적용,1세부 Fluoran계 감온색소에 가역적 감온변색성부여 위한 현색제, 상 전이물질, 용매 추가된 에멀전 중합 캡슐레이션 기술개발. 섬유가공 160℃ 내열 중합조건확립, 날염호에 투입, 세탁 ,마찰견뢰도 4급 이상, 의류제품 가능확인
- 기존 감온변색 캡슐의 멜라민을 Styrene으로 대체, 내열성과 견뢰도는 의류제품요구 기본성능 만족
■ 날염기법 적용, 군용 및 민수용 제품화를 위한 섬유소재적용 기술개발
- 기존 감온색소, 개발색소의 성능 분석 및 피드백
- 감온색소의 섬유 적용 위해 변색성, 색상, 견뢰도, Touch등 감안, 각종 첨가제의 Formulation레시피 정립
- Color paste 점도,Binder 등 최적 배합개발로 감온색소의 섬유적용 날염호 개발
- 다양한 색상구현 및 나일론, 면 공정기술개발로 일부 군용제품 및 일반의류제품용 섬유소재 적용기술 개발
- Semi-pilot공정기술개발로 감온색소 섬유 적용 위한 공정 조건 정립
■군용, 민수용 가변패턴 색상, 디자인 및 적용 시제품 개발
- 시장조사로 민수, 군수제품 조사 및 분석 완료
- 수집 자료 토대로 민수제품의 패턴 색상, 디자인 계획수립 . 군수제품은 감온변색 계절 부합온도 설정, 한국 환경부합 색상/패턴 전략 수립
- 민수7건 및 군수패턴 3건 디자인.10~15℃감온변화 작동 패턴 반영한 민수 완제품 9건, 군수 완제품 6건 샘플제작
(출처 : 보고서 요약서 3P)
Abstract
▼
Ⅳ. R & D results
■ Design, synthesis and discoloration characteristics of new thermochromic dye
- By using the framework of chromophore based on Leuco dye, various new thermochromic dye materials are designed and synthesized, and the results are derived by performing synthesis analysis, op
Ⅳ. R & D results
■ Design, synthesis and discoloration characteristics of new thermochromic dye
- By using the framework of chromophore based on Leuco dye, various new thermochromic dye materials are designed and synthesized, and the results are derived by performing synthesis analysis, optical characterization, and related experiments at different temperatures.
- A total of four different fluoran and two lactones were synthesized. In the case of four different fluoran, the originally planned monomer type was confirmed by structural analysis. The acid activator agent and low melting solvent were mixed to confirm the properties as a thermochromic dye.
- Set the method to exhibit a highly sensitive color change characteristic (Self-Thermochromic) without action of initiator (Color Developer) in response to the external stimulus as a research objective. Therefore, in this study, we conducted researches on the introduction of new parent and substituent groups for thermochromic discoloration of the Lactam ring, which is caused by the opening and closing of the Lactam ring, without the action of the initiator of the thermochromic material.
- Synthesis of five Betaine dyes synthesizing high sensitivity and reversible thermochromic characteristics using various scavengers and ligands. The result is obtained by structural analysis of materials, strenght analysis, or experiments according to temperature changes.
■ Synthesis of new thermochromic dye and scale up and development of commercialization formulation
- A new dye material was synthesized by diversifying fluoran system as a new thermochromic dye material and six new thermochromic dye materials (four kinds of fluoran and two kinds of lactone) were designed and synthesized by using chromophore framework based on Leuco dye, Synthetic and optical characterization, and associated experiments at different temperatures.
- Synthesis of novel Lactone / Aminofluoran, CVL and BDF gradation pigments Syntheses and Synthesis of Durability Additives (Durability enhancers were synthesized to minimize fading and discoloration when applied to thermochromic pigments which are structurally weak to light - Benzophenone, Triazole, Triazine)
- Secure of Lab scale up (500g) technology for four new developed dyes in 1-3 years and experiment to confirm the ability of heat development discoloration for five new developed dyes.
- Completion of sample delivery to second research consortium for production of prototype with self-synthesis result and registration for patent application of new heat-sensitive discoloration dye for 1st year
■ Microcapsulation technology to carry thermochromic dye
- Two types of non-melamine wall materials were investigated: polyurethane and styrene. In the first year, a basic study of polyurethane-based encapsulation was carried out to obtain capsules of about 5 μm in size. However, due to the complexity of the manufacturing process and the skin allergy problem in the prepolymer stage, it is expected that commercialization will be difficult. In the second year, the wall material is changed to styrene to study the encapsulation.
- In the second year, the basic preparation method of styrene encapsulation containing only dye was obtained. In the third year, a coloring agent for discoloration at a specific temperature and restoring the original color at other temperatures, We have developed a new encapsulation technology that includes all coloring agent, phase transition substances(paraffin wax) and solvents. In addition, the polymerization conditions to ensure the heat resistance at 160 ℃, which is the temperature required for fiber processing, were established, and the prepared capsules were put into a prescription for textile printing. After textile printing, washing and rubbing fastness measurement, it was confirmed that it is possible to develop clothes products with satisfactory result of grade 4 or higher.
- Through the 3-year encapsulation process, the melamine wall material, which is the limit of conventional thermo-sensitive color-change capsules for commercial clothing, was replaced with styrene. In terms of heat resistance and fastness.
- Through various changes in the process, the optimal solvent selection for a specific thermochromic dye, the optimum ratio of input to phase transition substances(paraffin wax) and a coloring agent in oil phase, and the optimum ratio of crosslinking agent for ensuring heat resistance were derived.
- In addition, the existing papers focus on applications other than fiber, such as construction, or encapsulation by agitation speed conditions. In this study, we have studied a wide range of applications such as heat resistance and fastness to textile commercialization, and this is considered to be a singular point.
■ Development of textile printing technology using thermochromic dye
- Through analyzing the performance of existing Thermochromic dyes, we tested compatibility, various fastness and found out the problem of existing Thermochromic dyes. So we found problem of new Thermochromic dyes in advance and developed foundation technology for application to fiber.
- As a result of analysis results of Existing Thermochromic dyes, It is not vivider than common pigment. Besides Its Colorfastness to light is not good. Due to using melamine based substance, thermochromic dyes have a problem which was detected formaldehyde.
- To apply thermochromic dyes to fiber, we developed thickener formulation for textile printing. Through Binder test, Fixing agent test, We optimized the system. Finally, thermochromic dyes’s depth of color was 10~20% upper than before. And it has improved on rubbing fastness as much as half grade. Also, we have optimized data about discoloration, the depth of color, fastness, and feeling.
- We compared new thermochromic dyes with existing thermochromic dyes. Consequently, new thermochromic dyes were a little bit dull in comparison with existing thermochromic dyes. But adjective quality was almost same.
- Also, We compounded fluorescent pigment + thermochromic dyes, and two types of thermochromic dyes. The latter’s Discoloration temperature is two step. So we can produce various colors. We applied to diverse fabric’s process. Consquently, we confirmed possibillity of product diversification of military and public purpose textile.
- Based on this foundation technology, We applied result of labatory test to semi-pilot process. And we set up process for new thermochromic dyes.
- Using thermochromic dyes, We developed two public purpose textile and military purpose textile. And it achieved upper than 4.0 grade about color fastness to washing and rubbing fastness. Using new thermochromic dyes, It was satisfied KC standard about formaldehyde.
■ Development of patterns and products using thermochromic dye
- Year one was spent creating the database of patterns and products in the civilian and military markets. The database will be utilized in the development of the civ/mil patterns and products. The database was created by researching the camouflage patterns and products through trend forecasting, conferences, and sample purchases.
- Strategy and planning of the patterns and products followed in year two using the data from the research in year one. For the civilian market, special attention was paid to use case where there were benefits of having a color changing product. For the military product, camouflage in varying seasons was of importance. In both cases, the requirements of the colors, pattern, design of the product was carefully planned to meet their goals. Also, the temperature settings for the different use cases had to be correctly selected in order for the colors changes to benefit the user.
- In accordance to the planning in year two, year three was spent designing the patterns on the fabric and the products themselves. The civilian products were designed for the outdoor, skiing, and exercising markets. In the military segment, the new camouflage patterns were developed for the mountainous regions of korea and applied to the combat uniform. Also, the color changing patterns were applied to other products that acted as covers for the solider and equipment.
- Color changing activation temperature was tested by using environmental and body temperature changes due to activity. After reviewing the results of the different civilian and military products developed, the conclusion can be made that color changing textiles have a potential in their designated markets. One major drawback was the lack of vibrant colors available and inconsistency of the color changes throughout the product.
(출처 : SUMMARY 10P)
목차 Contents
- 표지 ... 1
- 제 출 문 ... 2
- 보고서 요약서 ... 3
- 요 약 문 ... 5
- SUMMARY ... 10
- CONTENTS ... 16
- 목차 ... 18
- 제 1 장 연구개발과제의 개요 ... 19
- 제 1절 연구개발 목적 및 범위 ... 19
- 제 2절 연구개발의 필요성 ... 23
- 제 3절 연구개발의 추진체계 ... 31
- 제 2 장 국내외 기술개발 현황 ... 34
- 제 1절 국내 기술현황 ... 34
- 제 2절 국외 기술현황 ... 35
- 제 3절 국내외 지식재산권 현황 ... 36
- 제 4절 기술도입 가능성 ... 38
- 제 3 장 연구개발수행 내용 및 결과 ... 39
- 제 1절 신규 감온색소 설계, 합성 및 변색특성 개발 ... 39
- 제 2절 신규감온색소의 Scale-up 및 상용화 formulation 개발 ... 77
- 제 3절 감온색소의 마이크로캡슐레이션 기술개발 ... 121
- 제 4절 감온색소의 최적 날염기법 기술개발 ... 154
- 제 5 절 감온색소의 최적 가변패턴 디자인 개발 및 제품성 검토 ... 190
- 제 4 장 목표 달성도 및 관련분야에의 기여도 ... 225
- 제 1절 년차별 연구목표 및 달성도 ... 225
- 제 2절 관련분야 기술발전에의 기여도 ... 230
- 제 5 장 연구개발결과의 활용계획 ... 233
- 제 1절 추가연구의 필요성 및 타 연구에의 응용 ... 233
- 제 2절 기업화 추진방안 ... 239
- 제 6 장 연구개발과정에서 수집한 해외과학기술정보 ... 243
- 제 7 장 참고문헌 ... 247
- 끝페이지 ... 250
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