이 작품에 의해 지원 되었다는 갑니다 펀드 중국 농업 연구 시스템에 대 한 인 피와 잎 섬유 작물 (부여 번호 자동차-19), 중국 아카데미 농업 과학 및 기술 혁신 프로젝트 (보조금 번호 ASTIP-IBFC07), 혁신 펀드 동화 대학교에서 대학원 학생에 대 한 (번호 16 D 310107 부여), '핑 과학 및 기술 혁신 팀' (산업화 통합 생물학 degumming 인 피 섬유의 R & D 그룹), 중국 장학금 위원회.

1. 산화 Degumming 모시의
<ol><li>
솔루션 degumming 산화를 준비
	<ol>
<li>2 g H2O2, 1 g 알칼리 (Mg(OH)2 와 NaOH의 혼합물), 0.4 g 나5P3O10, 0.1 g 안트라퀴논, 그리고 0.2 g degumming 솔루션 HEDP 증류수 100 mL 물에 용 해.</li>
	</ol>
</li>
	<li>
모시의 산화 degumming
	<ol>
<li>담가 degumming 솔루션에서 10 g 원시 모시 고 샅 샅 히 뒤져 그것 아래 60 분 동안 85 ° C.</li>
		<li>125 ° c (0.6 k g의 압력) 온도 올리고 또 다른 60 분 샅 샅 히 뒤져. 주: 온도 높여에 설명에 대 한 토론을 참조 하십시오.</li>
	</ol>
</li>
	<li>
모시 섬유를 감소
	<ol>
<li>0.4 g NaHSO3 감소 솔루션을 준비 하 소 주 100ml 물에 용 해. 그런 다음 60 분 동안 90 ° C에서 줄이는 솔루션에서 degummed 섬유를 취급 합니다. 참고: carboxyl 그룹 및 알데하이드 그룹 셀 루 로스 산화 반응에서 생성 된 수소 결합의 감소 원인과 섬유 속성에 따라서 손상. Carboxyl 그룹을 변환 하 여 섬유의 재산 향상 시킬 수 그리고 수 산 기 그룹 알데하이드 그룹 다시.</li>
	</ol>
</li>
	<li>
후속 처리
	<ol>
<li>반죽 모시 섬유 이온된 물으로 깨끗이 씻는 다.</li>
		<li>15 분 동안 90 ° C에서 degumming 기름에 섬유를 담가 그리고 4 h (125 ° C)는 오븐에 섬유를 건조.</li>
	</ol>
</li>
</ol>2. Degumming 솔루션 속성 테스트
<ol><li>
Mg(OH)2 의 용 해도 시험
	<ol>
<li>2 세대 Mg(OH)2 증류수 100 mL 물에 용 해.</li>
		<li>별도로, 2 세대 Mg(OH)2 0.4 g 나5P3O10 등 0.2 g HEDP 완전히 녹는 degumming 첨가물 100 mL 해결책에서 녹.</li>
		<li>2.2.1 스텝과 2.2.2 85 ° c.에 설명 된 솔루션의 온도</li>
		<li>소 결 디스크 소화 Mg(OH)2 의 압축을 풉니다.</li>
		<li>다음 공식에 의해 Mg(OH)2 의 용 해도 계산. <img alt="Equation 2" src="/files/ftp_upload/56461/56461eq2.jpg"> 참고: 여기 m (g)는 소화 Mg(OH)2의 무게.</li>
	</ol>
</li>
	<li>
PH 값, ORP 값 및 degumming 솔루션의 잔여 H2O2 내용에 Mg(OH)2 대체 율의 영향 참고: ORP12,19 는 중요 한 물 화학 매개 변수 이며 주위 물의 산화 또는 감소 용량 측정 툴을 제공 한다. 강한 산화 속성 솔루션 높은 ORP 값을. Mg(OH)2 대체 율 (직물의 무게)에 10%의 총 알칼리 복용량에서 Mg(OH)2 로 대체 하는 NaOH의 몰 비율을 말합니다.<ol>
<li>각각 0%, 20%, 40%, 60%, 80%, 및 단계 1.1, 100%의 Mg(OH)2 대체 속도 degumming 솔루션을 준비 합니다.</li>
		<li>단계 2.2.1에서에서 설명한 degumming 솔루션에서 원시 모시를 담가.</li>
		<li>1.2 단계에 따라 degumming 프로세스를 시작 합니다.</li>
		<li>결합된 ORP 전극을 증류수로 세척 하 고 공기에서 건조. 다음 결합된 ORP 전극 미터 마다 10 분 담가 pH 값 마다 10 분을 읽는 degumming 솔루션에 pH 전극 미터 ORP 값을 읽는 degumming 솔루션에 젖어.</li>
		<li>22216 20087중국 표준 g B에 따라 KMnO4 적정 메서드에서 degumming 솔루션 마다 10 분의 H2O2 콘텐츠를 테스트 합니다.</li>
	</ol>
</li>
</ol>3. 모시 섬유 속성 테스트
<ol><li>
Degumming의 수익률
	<ol>
<li>다음 수식을 사용 하 여 degumming의 수익률을 계산: <img alt="Equation 3" src="/files/ftp_upload/56461/56461eq3.jpg"> 참고: 여기 w (g)는 섬유의 건조 중량 degumming; 후 W (g) degumming 전에 모시의 건조 중량 이다.</li>
	</ol>
</li>
	<li>
섬유의 잔여 잇 참고: 섬유의 잔여 잇 중국어 표준 5889-86에 따라 테스트 했다.<ol>
<li>무게 병에서 섬유 (약 5 g)의 건조 중량을 측정 하 고 150 mL NaOH 솔루션 (20 g/L)를 포함 (와 환류 응축 튜브) 플라스 크에 몰두.</li>
		<li>100 ° C의 온도 1 시간 동안이 온도에서 계속.</li>
		<li>NaOH 솔루션을 새로 고칩니다.</li>
		<li>100 ° C에 온도 2 시간에 대 한 유지.</li>
		<li>샘플 체에 섬유 씻어.</li>
		<li>병 무게에 섬유의 건조 무게를 측정 합니다.</li>
		<li>다음 수식을 사용 하 여 섬유의 잔여 잇을 계산. <img alt="Equation 4" src="/files/ftp_upload/56461/56461eq4.jpg"> 참고: 여기 m (g)는 섬유;의 건조 중량 (G) M NaOH 수 색 후 모시의 건조 중량 이다.</li>
	</ol>
</li>
	<li>
PD 시험 참고: 5888 8615중국 표준 g B에 따라 모시 섬유의 PD 값을 테스트 합니다.<ol>
<li>2:1 (v/v) 벤젠과 에틸 알코올 혼합물에 잠수 하 여 모시 섬유를 탈지 하십시오.</li>
		<li>실내 온도에 공기에서 용 매를 증발.</li>
		<li>샘플 짧은 조각으로 잘라 (1-2 m m, 20 ~ 23에 대 한 각 샘플에 대 한 mg)가 위를 사용 하 여.</li>
		<li>샘플 제어 습도 분위기에서 유지 (20 ± 2 ° C, 상대 습도 = 65 ± 2%) 무게 컨테이너 물 테스트 목적을 위해 요구 되는 물자를 제거 하기 전에 콘텐츠 평형을 도달할 때까지.</li>
		<li>집중된 한 질소 산, 98% 무수 ethylenediamine 뒤에 구리선 (0.5 m m 직경)을 담가. 다음, 구리과 립 증류수로 깨끗이 세척 하십시오.</li>
		<li>섬유 샘플 및 구리과 립 (상단)와 플라스틱 병에 넣어.</li>
		<li>플라스틱 병에 증류수 10 mL 물과 10 mL 1 mol/L cupriethylenediamine 솔루션을 추가 하 고 자기 볶음 바 준비 0.2 g/100 mL (약) 모시 섬유 cupriethylenediamine 솔루션을 사용 하 여 저 어.</li>
		<li>6.5 mL 모시 섬유 cupriethylenediamine 솔루션의 고유 점도 측정 하는 Ubbelohde 점도 계에 전송. 다음 수식으로 상대 점도 계산: <img alt="Equation 5" src="/files/ftp_upload/56461/56461eq5.jpg"> 참고: 여기 ηr 상대 점도, t (s)은 Ubbelohde 점도 계, t0를 통해 흐르는 모시 섬유 cupriethylenediamine 솔루션의 평균 시간 (s)는 0.5 mol/L cupriethylenediamine 솔루션 흐르는의 평균 시간입니다 Ubbelohde 점도 계입니다.</li>
		<li>다음 수식으로 모시 섬유의 PD 값을 계산: <img alt="Equation 6" src="/files/ftp_upload/56461/56461eq6.jpg"> 참고: 여기 [η]' 고유 점도 중국어 표준 GB 5888-86, 및 C에에서 테이블에서 [η] × C 값을 얻을 수 있습니다 ' 모시 섬유 cupriethylenediamine 솔루션의 농도 이다.</li>
	</ol>
</li>
	<li>
섬유의 선형 밀도
	<ol>
<li>다음 수식을 사용 하 여 섬유의 선형 밀도 계산. <img alt="Equation 7" src="/files/ftp_upload/56461/56461eq7.jpg"> 참고: 여기 Lc 절단 길이 (40 m m), n 은 섬유의 숫자 이며 G (g)는 섬유의 무게. 섬유의 선형 밀도 모시 (12%)의 공식 회복에서 1000 m 긴 섬유의 무게를 말합니다.</li>
	</ol>
</li>
	<li>
기계적 성질 시험
	<ol>
<li>표준 대기 조건에서 섬유 샘플을 equilibrate (T = 20 ± 2 ℃, RH = 65% ± 2%) 24 h에 대 한.</li>
		<li>끈기, 깨는 신장, 및 20 ° C, RH 65%, 및 0.3 cN/dtex의 사전 긴장의 다음 설정에서 섬유 강도 악기를 사용 하 여 섬유의 파열의 작업을 테스트 합니다. 20 mm 20 mm/min7,15에서 하단 클램프의 하강 속도에서 클램핑 거리를 설정 합니다.</li>
	</ol>
</li>
	<li>
Degumming 폐수의 COD 값
	<ol>
<li>15456 2008 '산업 순환 냉각 물-대구-칼륨과 망간 산 염 방법의 결정'7,15중국 표준 GB/T에 따르면 degumming 폐수의 COD를 테스트 합니다.</li>
	</ol>
</li>
	<li>
XRD 테스트
	<ol>
<li>X 선 회절을 사용 하 여 섬유의 결정을 얻을. 기록 XRD 패턴 2θ 흑연 단색, λ에 Cu Kα 방사선 diffractometer와 5-60 ° = = 0.154 nm (40 kV, 200 mA).</li>
	</ol>
</li>
	<li>
FTIR 분석
	<ol>
<li>분석기를 사용 하 여 섬유의 연결 패턴을 가져옵니다. 30, 스캔 시간 설정 4000-400 c m-1, 8 cm-1에 해상도에서 범위. FT-적외선 분석을 사용 하 여 치료 섬유에서 화학 기능적인 그룹을 결정 합니다.</li>
	</ol>
</li>
</ol>

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W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Alkali+Source+Used+in+the+Oxidation+Degumming+of+Ramie.">Alkali Source Used in the Oxidation Degumming of Ramie.</a> Text Res J. 87 (10), 1155-1164 (2017).</li><li>Gorski, D., Engstrand, P., Hill, J., Axelsson, P., Johansson, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mg(OH)2-based+hydrogen+peroxide+refiner+bleaching:+influence+of+extractives+content+in+dilution+water+on+pulp+properties+and+energy+efficiency.">Mg(OH)2-based hydrogen peroxide refiner bleaching: influence of extractives content in dilution water on pulp properties and energy efficiency.</a> Appita Journal. 63 (3), 218-225 (2010).</li><li>Leduc, C., Martel, J., Danea, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Efficiency+and+effluent+characteristic+from+Mg(OH)2-based+hydrogen+peroxide+bleaching+of+high-yield+pulps+and+deinked+pulp.">Efficiency and effluent characteristic from Mg(OH)2-based hydrogen peroxide bleaching of high-yield pulps and deinked pulp.</a> Cellulose Chemistry &amp; Technology. 44 (7-8), 271-276 (2010).</li></ol>

저자는 공개 없다.

Mg(OH)2 대체 속도 반응 온도 설정이이 프로토콜의 핵심 이었다. Mg(OH)2 대체 속도 pH 값 및 따라서 degumming 솔루션의 산화 능력을 좌우할 수 있다. 모시 degumming에 대 한 최고의 Mg(OH)2 대체 율은 20%, 셀 루 로스 20%, 대체 율에서 충분 한 보호를 받을 수 있기 때문에 잔여 잇 (낮은 DP 값 및 결정)의 과도 한 양의 섬유에서 유지 될 것 20% (그림 4A) 이상 대체 속도?...

일반적으로 '중국 잔디'로 알려진 모시는 누구의 섬유 섬유 산업1,2에 대 한 훌륭한 자료로 사용 될 수 있다 다년생 나물 이다. 그것은 네이티브 중국; 주요 경제 작물 중 하나 중국에는 모시의 생산 세계1,2총 생산량의 90% 이상을 차지 하고있다. 모시 섬유는 거의 부드러운 외관3,4광택 강한 고 긴 식물 섬유 중 하나입니다. 모시 섬유의 긴 길이 거의 인 피 섬유에서 볼 수 있는 단일 섬유 회전에 적합 하 게. 모시 섬유에서 만든 섬유 등3,4 , 환기, 항균, 우수한 열 전도성, 차가움 등 많은 우수한 속성을가지고
셀 룰 로스 모시 섬유의 주요 구성 요소 이며,5,6잇 몸 모시, 펙 틴, 리그 닌, 물 녹는 재료, 다른 구성 요소 정의 됩니다. 모시 섬유는 화학 시 약,5,6degumming로 정의 된 프로세스에 포함 된 솔루션에서 잇을 용 해 하 여 추출할 수 있습니다. 존재 하는 모시 섬유 추출의 주로 두 가지 방법: 화학 degumming 및 바이오 degumming. 에너지 소비, 시간 소모, 그리고 대구에 전통적인 화학 degumming degumming 폐수의 가치는 오히려 높은, 셀 룰 로스로 섬유 6 ~ 8 h7,8에 대 한 높은 압력에서 집중된 NaOH에 원시 모시를 수 색 하 여 추출 . 또한, 바이오 degumming 모시 섬유 추출에 대 한 환경 친화적인 옵션입니다. 그럼에도 불구 하 고, 가혹한 반응 조건 및 정교한 장비는 더 산업 응용9,10을 억제합니다. 그러므로, 귀중 한 선물 알칼리 수소 과산화 수소와 산화 degumming 하며 그것에 대 한 초점을 대체 응용 프로그램 짧은 degumming 시간과 낮은 degumming 온도11,12. 그러나,는 과산화물의 강력한 산화 능력 때문 상당한 셀 룰 로스 분해 과정에서 degumming, 섬유 속성13,14에 큰 손상을 일으킬 수 있습니다 발생할 수 있습니다. 이것은 알칼리 과산화 수소 산화 degumming 모시의의 가장 큰 단점입니다.
이전 학문에서는, 모시 섬유는 수산화 나트륨15에서만 지원 되는 알칼리 과산화 수소 시스템에서 추출 되었다. 그러나, 때문에 수산화 나트륨의 강한 알칼리, 과산화 수소의 산화 반응 속도 제어 하기 어려운 되었고 따라서 치료 섬유7에 큰 피해 발생. 모시 섬유의 속성, 개선 하기 위해 알칼리 상태를 제공 하 고 알칼리 과산화 수소 시스템16 의 pH 값을 버퍼를 제어 릴리스 알칼리 소스, 수산화 나트륨, 수산화 마그네슘의 구성 되는이 연구에 사용 된 , 17.
이 기술 뒤에 근거는 다음과 같이 설명할 수 있습니다. 수산화 마그네슘 증된 물에 약간 용 해 이며 아- 의 소비와 degumming 솔루션으로 점차적으로 해산 하 고 적절 한 범위18에서 pH 값 및 따라서 degumming 솔루션의 산화 능력을 유지 수 있습니다. 수산화 마그네슘의 대체 율 (SR) 10%, 총 알칼리 량에서 수산화 마그네슘으로 대체 하는 NaOH의 몰 비율으로 정의 되 고 대체 속도 다음 식에 의해 계산할 수 있다. 또한, Mg2 + 방지할 수 있다 셀 루 로스 저하 산화19,20이상으로 인 한.
<img alt="Equation 1" src="/files/ftp_upload/56461/56461eq1.jpg">
여기, M2 (g)은 Mg(OH)2의 무게, M1 (g)은 NaOH의 무게, 40은 NaOH의 분자량, 58은 Mg(OH)2의 분자량, 2는 Mg(OH)2, OHs의 수 그리고 SR은 대체.
이 프로토콜의 기술 추출, 표백, 및 식물 재료의 알칼리 과산화 수소 시스템에서 수정 확장할 수 있습니다. 그러나, 그것은 알칼리 과산화 수소 시스템의 pH 값과 반응 온도 선택이 기술21에 대 한 열쇠는 주목 해야 합니다. 알칼리 과산화 수소 시스템의 pH 값 대체 율17를 변경 하 여 조정할 수 있습니다. PH 값과 따라서 산화 능력 알칼리 과산화 수소 시스템의 대체 율의 증가 함께 감소 한다. 반응 온도 85 ° C에서 설정 되어, 자유 라 디 칼 반응 시스템에서 주요 역할을 담당 하며 시스템의 강한 산화 재료; 해산 적합 125 ° C에서 반응 온도 설정 하면 자유 라 디 칼 반응을 저해 하 고 시스템을19표백에 적합 하 게 시스템에 존재 하는 많은 양의 후.

<table>
	<tbody>
		<tr>
			<td>Hydrogen peroxide, 30%</td>
			<td>Fisher Scientific</td>
			<td>H325-100</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Magnesium hydroxide, 99%</td>
			<td>Fisher Scientific</td>
			<td>AA1236722</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium hydroxide</td>
			<td>Fisher Scientific</td>
			<td>S318-1</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium bisulfite</td>
			<td>Fisher Scientific</td>
			<td>S654-500</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Sodium tripolyphosphate</td>
			<td>Fisher Scientific</td>
			<td>AC218675000</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Anthraquinone, &#62;98%</td>
			<td>Fisher Scientific</td>
			<td>AC104930500</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>1-Hydroxy Ethylidene-1,1-Diphosphonic Acid</td>
			<td>Fisher Scientific</td>
			<td>50-901-10243</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Degumming oil</td>
			<td>Minglong auxiliaries limited liability company, Yiyang, Hunan,China</td>
			<td>&#8212;&#8212;</td>
			<td>Chemical for degumming</td>
		</tr>
		<tr>
			<td>Ethyl alcohol</td>
			<td>Fisher Scientific</td>
			<td>A962-4</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Benzene</td>
			<td>Fisher Scientific</td>
			<td>AA43817AE</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Copper wire,0.5mm (0.02in) dia</td>
			<td>Fisher Scientific</td>
			<td>AA10783H4</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Cupriethylenediamine solution 1mol/L</td>
			<td>Fisher Scientific</td>
			<td>24991</td>
			<td>Chemical for testing, caution toxic</td>
		</tr>
		<tr>
			<td>Nitric acid (65% ~68% )</td>
			<td>Fisher Scientific</td>
			<td>A200-612GAL</td>
			<td>Chemical for testing, caution</td>
		</tr>
		<tr>
			<td>Ethylenediamine</td>
			<td>Fisher Scientific</td>
			<td>AC118420100</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Potassium permanganate</td>
			<td>Fisher Scientific</td>
			<td>P279-500</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Sulphuric acid</td>
			<td>Fisher Scientific</td>
			<td>A300C-212</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Silver sulfate</td>
			<td>Fisher Scientific</td>
			<td>S190-25</td>
			<td>Chemical for testing</td>
		</tr>
		<tr>
			<td>Raw ramie</td>
			<td>Guangyuan limited liability company, Changde, Hunan,China</td>
			<td>&#8212;&#8212;</td>
			<td>Raw materials</td>
		</tr>
		<tr>
			<td>Electric-heated&#160;thermostatic&#160;water&#160;bath</td>
			<td>Senxin Experiment equipment limited liability company,Shanghai,China</td>
			<td>DK-S28</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>High temperature lbaorator dyeing machine</td>
			<td>Shanghai Longda chemcials Crop.</td>
			<td>RY-1261</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>Thermometer</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>100 &#176;C</td>
			<td>Equipments for degumming</td>
		</tr>
		<tr>
			<td>Vacuum suction machine</td>
			<td>Yukang KNET ,Shanghai,China</td>
			<td>SHB-IIIA</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Suction flask</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>1000mL</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Sand-core funnels</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>35mL</td>
			<td>Equipments for testing Mg(OH)2 solublity</td>
		</tr>
		<tr>
			<td>Oxidation reduction potential meter</td>
			<td>Dapu instrument, Shanghai, China</td>
			<td>MODEL 421</td>
			<td>Equipments for testing ORP value</td>
		</tr>
		<tr>
			<td>pH meter</td>
			<td>Hanna instruments,Beijing,China</td>
			<td>HI 98129</td>
			<td>Equipments for testing pH value</td>
		</tr>
		<tr>
			<td>Acid burette</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>50mL</td>
			<td>Equipments for testing H2O2 content</td>
		</tr>
		<tr>
			<td>Flask</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL/500mL</td>
			<td>Equipments for testing H2O2 content;&#160; residual gums content</td>
		</tr>
		<tr>
			<td>Electric furnace</td>
			<td>Jiangyi Experiment instruments limited liability company,Shanghai,China</td>
			<td>800-2000W</td>
			<td>Equipments for testing residual gums content</td>
		</tr>
		<tr>
			<td>Reflux condensing tube</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing residual gums content; COD value</td>
		</tr>
		<tr>
			<td>Fiber cutter (40mm)</td>
			<td>Changzhou No.2 Textile Machine Co.,Ltd</td>
			<td>Y171A</td>
			<td>Equipments for testing fiber density</td>
		</tr>
		<tr>
			<td>Ostwald viscometer</td>
			<td>Taizhou, jiaojiang, glass instruments company</td>
			<td>0.6mm</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Spherical fat extractor</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Soxhlet extractor</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL</td>
			<td>Equipments for testing fiber PD value</td>
		</tr>
		<tr>
			<td>Torsion&#160;balance</td>
			<td>Liangping instrucments Co.,Ltd,Shanghai, China</td>
			<td>JN-B</td>
			<td>Equipments for testing fiber density</td>
		</tr>
		<tr>
			<td>Fiber strength instrument</td>
			<td>Xinxian instruments, shanghai,China</td>
			<td>XQ-2</td>
			<td>Equipments for testing fiber tensile property</td>
		</tr>
		<tr>
			<td>Tension clamp</td>
			<td>Depu textile technology Co.,Ltd, Changzhou, jiangsu, China</td>
			<td>0.3cN/dtex</td>
			<td>Equipments for testing fiber tensile property</td>
		</tr>
		<tr>
			<td>COD&#160;thermostatic&#160;heater</td>
			<td>Qiangdao Xuyu environment protection technology Lit company</td>
			<td>DL-801A</td>
			<td>Equipments for testing COD value</td>
		</tr>
		<tr>
			<td>FTIR</td>
			<td>Thermo Fisher, America</td>
			<td>Nicolet</td>
			<td>FTIR analysis</td>
		</tr>
		<tr>
			<td>XRD</td>
			<td>Rigaku, Japan</td>
			<td>D/max-2550 PC</td>
			<td>XRD analysis</td>
		</tr>
		<tr>
			<td>Electronic balance</td>
			<td>Shanghai jingtian Electronic instrument Co.,Ltd</td>
			<td>FA2004A</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Drying oven</td>
			<td>Tonglixinda&#160; instruments, Tianjin,China</td>
			<td>101-2AS</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Weighing bottle</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>50x30</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Beaker</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>500mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Sample sieve</td>
			<td>Xiaojin hardware instruments Co.,Ltd, Shangyu, Zhejiang</td>
			<td>120 mesh</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Glass rod</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>&#8212;&#8212;</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Cylinder</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>250mL, 50mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Pipette</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>5mL, 10mL</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Rubber&#160;suction&#160;bulb</td>
			<td>Sichuan Shubo (group)Co.,Ltd</td>
			<td>&#8212;&#8212;</td>
			<td>Generral equipments</td>
		</tr>
		<tr>
			<td>Orign</td>
			<td>OriginLab</td>
			<td>8.0</td>
			<td>Software for figure drawing</td>
		</tr>
	</tbody>
</table>

extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source

이 프로토콜에서는 알칼리 과산화 수소 시스템 제어 릴리스 알칼리 소스에서 지 원하는 원시 모시를 수 색 하 여 모시 섬유 추출 하는 방법을 보여 줍니다. 모시에서 추출한 섬유 매우 중요 섬유 재료의 종류 이다. 이전 학문에서는, 모시 섬유는 수산화 나트륨 에서만 지원 되는 알칼리 과산화 수소 시스템에서 추출 했다. 그러나, 때문에 수산화 나트륨의 강한 알칼리, 과산화 수소의 산화 반응 속도 제어 하기 어려운 되었고 치료 섬유에 따라서 큰 피해 발생. 이 프로토콜에서 수산화 나트륨과 수산화 마그네슘의 구성 되는 제어 릴리스 알칼리 소스는 알칼리 상태를 제공 하 고 알칼리 수소 peroxidesystem의 pH 값을 버퍼링 하는 데 사용 됩니다. 수산화 마그네슘의 대체 율 과산화 수소 시스템의 pH 값을 조정할 수 있으며 섬유 속성에 큰 영향. PH 값과 oxidation-reduction 잠재력 (ORP) 값, 알칼리 과산화 수소 시스템의 산화 능력을 나타내는 pH 미터, ORP 미터, 각각 사용 하 여 감시 되었다. 추출 과정 및 섬유 추출 후 폐수의 화학적 산소 수요 (대구) 값 중 알칼리 과산화 수소 시스템에서 과산화 수소 잔류 콘텐츠 KMnO4 적정 방법으로 테스트 합니다. 정밀 전자 저울을 사용 하 여 섬유의 수확량을 측정 하 고 잔여 잇 몸 섬유의 화학 분석 방법에 의해 테스트 됩니다. 섬유의 중 합도 (PD 값) 내장 점도 방법 Ubbelohde 점도 계를 사용 하 여 테스트 됩니다. 섬유, 끈기, 신장, 파열 등의 인장 속성 섬유 강도 악기를 사용 하 여 측정 됩니다. 푸리에 변환 적외선 분광학 그리고 x 선 회절 기능 그룹 및 섬유의 크리스탈 재산을 특성화 하는 데 사용 됩니다. 이 프로토콜 제어 릴리스 알칼리 소스 알칼리 과산화 수소 시스템에서 추출 하는 섬유의 속성을 향상 시킬 수 있는 증명 한다.

증류수 및 degumming 솔루션 Mg(OH)2 의 용 해도 공부 했다 (그림 1). PH 값 및 degumming 솔루션의 ORP 값 (그림 2) Mg(OH)2 대체 속도의 효과 테스트 했다. Degumming 수율 및 섬유2 대체 율은 다양 한 Mg(OH)에서 반죽의 잔여 잇 몸 (그림 3)를 계산 합니다. DP 값, 화도, (그림 4), ?...

Watch this Scientific Journal Video about Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source at JoVE.com

Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

알칼리 과산화 수소 시스템 제어 릴리스 알칼리 소스에서 지 원하는 모시 섬유의 추출

여기는 알칼리 과산화 수소 시스템 제어 릴리스 알칼리 소스에서 지 원하는 모시 섬유의 적 출을 위한 프로토콜이입니다.

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a ...

extraction-ramie-fiber-alkali-hydrogen-peroxide-system-supported

Research

JoVE Journal

Chemistry

11.3K 조회수.  Donghua University. 여기는 알칼리 과산화 수소 시스템 제어 릴리스 알칼리 소스에서 지 원하는 모시 섬유의 적 출을 위한 프로토콜이입니다.

비디오: Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

Exfoliation of Egyptian Blue and Han Blue, Two Alkali Earth Copper Silicate-based Pigments

In a visualized example of the ancient past connecting with modern times, we describe the preparation and exfoliation of CaCuSi4O10 and BaCuSi4O10, the colored components of the historic Egyptian blue and Han blue pigments. The bulk forms of these materials are synthesized by both melt flux and solid-state routes, which provide some control over the crystallite size of the product. The melt flux process is time intensive, but it produces relatively large crystals at lower reaction temperatures. In comparison, the solid-state method is quicker yet requires higher reaction temperatures and yields smaller crystallites. Upon stirring in hot water, CaCuSi4O10 spontaneously exfoliates into monolayer nanosheets, which are characterized by TEM and PXRD. BaCuSi4O10 on the other hand requires ultrasonication in organic solvents to achieve exfoliation. Near infrared imaging illustrates that both the bulk and nanosheet forms of CaCuSi4O10 and BaCuSi4O10 are strong near infrared emitters. Aqueous CaCuSi4O10 and BaCuSi4O10 nanosheet dispersions are useful because they provide a new way to handle, characterize, and process these materials in colloidal form.

The preparation and exfoliation of CaCuSi4O10&#160;and BaCuSi4O10 are described. Upon stirring in hot water, CaCuSi4O10 spontaneously exfoliates into monolayers, whereas BaCuSi4O10&#160;requires ultrasonication in organic solvents. Near infrared (NIR) imaging illustrates the NIR emission properties of these materials, and aqueous dispersions of these nanomaterials are useful for solution processing.

이집트 블루와 한 블루, 알칼리 지구 구리 실리케이트 계 안료의 각질 제거

In a visualized example of the ancient past connecting with modern times, we describe the preparation and exfoliation of CaCuSi4O10 and BaCuSi4O10, the ...

연구

화학

Preparing Adherent Cells for X-ray Fluorescence Imaging by Chemical Fixation

X-ray fluorescence imaging allows us to non-destructively measure the spatial distribution and concentration of multiple elements simultaneously over large or small sample areas. It has been applied in many areas of science, including materials science, geoscience, studying works of cultural heritage, and in chemical biology. In the case of chemical biology, for example, visualizing the metal distributions within cells allows us to study both naturally-occurring metal ions in the cells, as well as exogenously-introduced metals such as drugs and nanoparticles. Due to the fully hydrated nature of nearly all biological samples, cryo-fixation followed by imaging under cryogenic temperature represents the ideal imaging modality currently available. However, under the circumstances that such a combination is not easily accessible or practical, aldehyde based chemical fixation remains useful and sometimes inevitable. This article describes in as much detail as possible in the preparation of adherent mammalian cells by chemical fixation for X-ray fluorescent imaging.

Here, we present a protocol on how to determine the quantity and distribution of metals in a sample using synchrotron X-ray fluorescence. We focus on adherent cells, and describe the chemical fixation method to prepare this sample. We then describe how to mount and image the sample using synchrotron X-rays.

화학 고정하여 X-ray 형광 이미징 부착 세포를 준비

X-ray fluorescence imaging allows us to non-destructively measure the spatial distribution and concentration of multiple elements simultaneously over ...

Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. Herein, nitrogen is presented as a novel supercritical drying fluid for specialized applications such as in the processing of reactive porous materials, where carbon dioxide and other fluids are not appropriate due to their higher chemical reactivity. Nitrogen exhibits similar physical properties in the near-critical region of its phase diagram as compared to carbon dioxide: a widely tunable density up to ~1 g ml-1, modest critical pressure (3.4 MPa), and small molecular diameter of ~3.6 &#197;. The key to achieving a high solvation power of nitrogen is to apply a processing temperature in the range of 80-150 K, where the density of nitrogen is an order of magnitude higher than at similar pressures near ambient temperature. The detailed solvation properties of nitrogen, and especially its selectivity, across a wide range of common target species of extraction still require further investigation. Herein we describe a protocol for the supercritical nitrogen processing of porous magnesium borohydride.

Nitrogen is an effective supercritical fluid for extraction or drying processes due to its small molecular size, high density in the near-liquid supercritical regime, and chemical inertness. We present a supercritical nitrogen drying protocol for the purification treatment of reactive, porous materials.

반응성이 있음 다공성 물질의 정제를위한 초 임계 질소 처리

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. ...

A Simple, Low-cost, and Robust System to Measure the Volume of Hydrogen Evolved by Chemical Reactions with Aqueous Solutions

There is a growing research interest in the development of portable systems which can deliver hydrogen on-demand to proton exchange membrane (PEM) hydrogen fuel cells. Researchers seeking to develop such systems require a method of measuring the generated hydrogen. Herein, we describe a simple, low-cost, and robust method to measure the hydrogen generated from the reaction of solids with aqueous solutions. The reactions are conducted in a conventional one-necked round-bottomed flask placed in a temperature controlled water bath. The hydrogen generated from the reaction in the flask is channeled through tubing into a water-filled inverted measuring cylinder. The water displaced from the measuring cylinder by the incoming gas is diverted into a beaker on a balance. The balance is connected to a computer, and the change in the mass reading of the balance over time is recorded using data collection and spreadsheet software programs. The data can then be approximately corrected for water vapor using the method described herein, and parameters such as the total hydrogen yield, the hydrogen generation rate, and the induction period can also be deduced. The size of the measuring cylinder and the resolution of the balance can be changed to adapt the setup to different hydrogen volumes and flow rates.

The study of methods to generate on-demand hydrogen for fuel cells continues to grow in importance. However, systems to measure hydrogen evolution from the reaction of chemicals with water can be complicated and expensive. This article details a simple, low-cost, and robust method to measure the evolution of hydrogen gas.

간단한, 낮은 비용, 강력한 시스템 수성 솔루션과 화학 반응에 의해 진화 수소의 양을 측정하는

There is a growing research interest in the development of portable systems which can deliver hydrogen on-demand to proton exchange membrane (PEM) ...

Real-time Breath Analysis by Using Secondary Nanoelectrospray Ionization Coupled to High Resolution Mass Spectrometry

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental exposure in a non-invasive manner. In this work, we present a protocol to characterize the exhaled VOCs in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry (Sec-nanoESI-HRMS). The homemade Sec-nanoESI source was readily set up based on a commercial nanoESI source. Hundreds of peaks were observed in the background-subtracted mass spectra of exhaled breath, and the mass accuracy values are -4.0-13.5 ppm and -20.3-1.3 ppm in the positive and negative ion detection modes, respectively. The peaks were assigned with accurate elemental composition according to the accurate mass and isotopic pattern. Less than 30 s is used for one exhalation measurement, and it takes approximately 7 min for six replicated measurements.

A protocol for characterizing chemical composition of exhaled breath in real time by using secondary nanoelectrospray ionization coupled to high resolution mass spectrometry is demonstrated.

고 분해능 질량 분석을 결합 하는 보조 Nanoelectrospray 이온화를 사용 하 여 실시간 호흡 분석

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental ...

Photoelectron Imaging of Anions Illustrated by 310 Nm Detachment of F&#8722;

Anion photoelectron imaging is a very efficient method for the study of energy states of bound negative ions, neutral species and interactions of unbound electrons with neutral molecules/atoms. State-of-the-art in vacuo anion generation techniques allow application to a broad range of atomic, molecular, and cluster anion systems. These are separated and selected using time-of-flight mass spectrometry. Electrons are removed by linearly polarized photons (photo detachment) using table-top laser sources which provide ready access to excitation energies from the infra-red to the near ultraviolet. Detecting the photoelectrons with a velocity mapped imaging lens and position sensitive detector means that, in principle, every photoelectron reaches the detector and the detection efficiency is uniform for all kinetic energies. Photoelectron spectra extracted from the images via mathematical reconstruction using an inverse Abel transformation reveal details of the anion internal energy state distribution and the resultant neutral energy states. At low electron kinetic energy, typical resolution is sufficient to reveal energy level differences on the order of a few millielectron-volts, i.e., different vibrational levels for molecular species or spin-orbit splitting in atoms. Photoelectron angular distributions extracted from the inverse Abel transformation represent the signatures of the bound electron orbital, allowing more detailed probing of electronic structure. The spectra and angular distributions also encode details of the interactions between the outgoing electron and the residual neutral species subsequent to excitation. The technique is illustrated by the application to an atomic anion (F&#8722;), but it can also be applied to the measurement of molecular anion spectroscopy, the study of low lying anion resonances (as an alternative to scattering experiments) and femtosecond (fs) time resolved studies of the dynamic evolution of anions.

Here, we present a protocol for photoelectron imaging of anionic species. Anions generated in vacuo and separated by mass spectrometry are probed using velocity mapped photoelectron imaging, providing details of anion and neutral energy levels, anion and neutral structure and the nature of the anion electronic state.

F− 의 310 Nm 분리에 의해 설명 하는 음이온의 광전자 이미징

Anion photoelectron imaging is a very efficient method for the study of energy states of bound negative ions, neutral species and interactions of unbound ...

Extraction of Lignin with High &#946;-O-4 Content by Mild Ethanol Extraction and Its Effect on the Depolymerization Yield

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the emerging elegant procedures to obtain specific aromatic products rely on the lignin substrate having a high content of the readily cleavable &#946;-O-4 linkage as present in the native lignin structure. This provides a miss-match with typical technical lignins that are highly degraded and therefore are low in &#946;-O-4 linkages. Therefore, the extraction yields, and the quality of the obtained lignin are of utmost importance to access new lignin valorization pathways. In this manuscript, a simple protocol is presented to obtain lignins with high &#946;-O-4 content by relatively mild ethanol extraction that can be applied to different lignocellulose sources. Furthermore, analysis procedures to determine the quality of the lignins are presented together with a depolymerization protocol that yields specific phenolic 2-arylmethyl-1,3-dioxolanes, which can be used to evaluate the obtained lignins. The presented results demonstrate the link between lignin quality and potential for the lignins to be depolymerized into specific monomeric aromatic chemicals. Overall, the extraction and depolymerization demonstrates a trade-off between the lignin extraction yield and the retention of the native aryl-ether structure and thus the potential of the lignin to be used as the substrate for the production of chemicals for higher-value applications.

Here, we present a protocol to perform ethanol extraction of lignin from several biomass sources. The effect of the extraction conditions on the lignin yield and &#946;-O-4 content are presented. Selective depolymerization is performed on the obtained lignins to obtain high aromatic monomer products.

온화한 에탄올 추출 및 Depolymerization 수율에 미치는 영향에 의해 높은 β-O-4 콘텐츠 리그 닌의 추출

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the ...

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

We describe a method to produce U2O5 films in situ using the Labstation, a modular machine developed at JRC Karlsruhe. The Labstation, an essential part of the Properties of Actinides under Extreme Conditions laboratory (PAMEC), allows the preparation of films and studies of sample surfaces using surface analytical techniques such as X-ray and ultra-violet photoemission spectroscopy (XPS and UPS, respectively). All studies are made in situ, and the films, transferred under ultra-high vacuum from their preparation to an analyses chamber, are never in contact with the atmosphere. Initially, a film of UO2 is prepared by direct current (DC) sputter deposition on a gold (Au) foil then oxidized by atomic oxygen to produce a UO3 film. This latter is then reduced with atomic hydrogen to U2O5. Analyses are performed after each step involving oxidation and reduction, using high-resolution photoelectron spectroscopy to examine the oxidation state of uranium. Indeed, the oxidation and reduction times and corresponding temperature of the substrate during this process have severe effects on the resulting oxidation state of the uranium. Stopping the reduction of UO3 to U2O5 with single U(V) is quite challenging; first, uranium-oxygen systems exist in numerous intermediate phases. Second, differentiation of the oxidation states of uranium is mainly based on satellite peaks, whose intensity peaks are weak. Also, experimenters should be aware that X-ray spectroscopy (XPS) is a technique with an atomic sensitivity of 1% to 5%. Thus, it is important to obtain a complete picture of the uranium oxidation state with the entire spectra obtained on U4f, O1s, and the valence band (VB). Programs used in the Labstation include a linear transfer program developed by an outside company (see Table of Materials) as well as data acquisition and sputter source programs, both developed in-house.

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

This protocol presents the preparation of U2O5 thin films obtained in situ under ultra-high vacuum. The process involves oxidation and reduction of UO2 films with atomic oxygen and atomic hydrogen, respectively.

UO2 증 착 직류 스퍼터 링 및 연속 산화와 산소 원자와 원자 수소 감소를 통해 U2O5 영화 준비

We describe a method to produce U2O5 films in situ using the Labstation, a modular machine developed at JRC Karlsruhe. The Labstation, an essential part ...

Experimental Methods for Efficient Solar Hydrogen Production in Microgravity Environment

Long-term space flights and cis-lunar research platforms require a sustainable and light life-support hardware which can be reliably employed outside the Earth's atmosphere. So-called 'solar fuel' devices, currently developed for terrestrial applications in the quest for realizing a sustainable energy economy on Earth, provide promising alternative systems to existing air-revitalization units employed on the International Space Station (ISS) through photoelectrochemical water-splitting and hydrogen production. One obstacle for water (photo-) electrolysis in reduced gravity environments is the absence of buoyancy and the consequential, hindered gas bubble release from the electrode surface. This causes the formation of gas bubble froth layers in proximity to the electrode surface, leading to an increase in ohmic resistance and cell-efficiency loss due to reduced mass transfer of substrates and products to and from the electrode. Recently, we have demonstrated efficient solar hydrogen production in microgravity environment, using an integrated semiconductor-electrocatalyst system with p-type indium phosphide as the light-absorber and a rhodium electrocatalyst. By nanostructuring the electrocatalyst using shadow nanosphere lithography and thereby creating catalytic 'hot spots' on the photoelectrode surface, we could overcome gas bubble coalescence and mass transfer limitations and demonstrated efficient hydrogen production at high current densities in reduced gravitation. Here, the experimental details are described for the preparations of these nanostructured devices and further on, the procedure for their testing in microgravity environment, realized at the Bremen Drop Tower during 9.3 s of free fall.

Efficient solar-hydrogen production has recently been realized on functionalized semiconductor-electrocatalyst systems in a photoelectrochemical half-cell in microgravity environment at the Bremen Drop Tower. Here, we report the experimental procedures for manufacturing the semiconductor-electrocatalyst device, details of the experimental set-up in the drop capsule and the experimental sequence during free fall.

미세 중력 환경에서 효율적인 태양 수소 생산을위한 실험 방법

Long-term space flights and cis-lunar research platforms require a sustainable and light life-support hardware which can be reliably employed outside the ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

표면 유기 금속 화학의 방법론을 사용하여 실리카 지원 촉매에 의해 이민 대사

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...