총통, 첸, 그리고 왕 박사 학위를 방문하는 동안이 작품은 실시 하였다 미국 산림청, 임산물 연구소 (FPL), 매디슨, 위스콘신,에서와 주홍의 공식적인 정부 시간에 학생. 이 작품은 부분적으로 USDA 농업 및 식품 연구 이니셔티브 (AFRI) 경쟁 그랜트 (제 2011-67009-20056), 중국 국가 임업 국 (프로젝트 제 2015-4-54), 국립 자연 과학 재단에 의해 지원되었다 중국 (프로젝트 번호 31470599), 중국의 광저우 엘리트 프로젝트, 중국 장학 기금. 이 프로그램에서 자금 조달이 가능 FPL에서 총통, 첸, 그리고 왕의 방문 약속을했다.

참고 : 표백 유칼립투스 크라프트 펄프 (BEP) 및 상업 소스의 표백 혼합 활엽수 크라프트 펄프 (UMHP) 섬유는 CNC 및 CNF 제조 원료로 사용 하였다. 구입 한 상용 말레 산 가수 분해에 사용 하였다. 가수 분해 조건은 각각 BEP 및 UMHP 들어, 60 분, 120 분, 120 ℃ (상압에서의 비점 없음) 100 ℃에서 60 중량 %의 산 농도였다. 집중 디카 르 복실 산 솔루션 1. 준비 <ol><li> 가열판 약 85 ° C에서 액체 글리세린 욕에서 다중 구 플라스크에 (DI) 탈 이온수 40 mL의 열. </li><li> 자기 교반하면서 60 중량 %의 용액을 플라스크에 60g의 무수 말레 산을 추가한다. 이전에보고 된 15 산 용액의 농도를 이용하여, 특정 질량 농도의 산 용액을 물과 아세트산의 요구량을 계산한다. </li><li> 드에 대한 해결책을 가열(높아 디카 르 복실 산 농도 비등) 100 또는 120 ° C의 온도를 희망하는 가수. </li></ol> 2. 가수 분해 반응 <ol><li> 산 용액의 온도에서 일단 연속 교반하면서 80 mL의 디카 르 복실 산 용액 (1.1)로 BEP 또는 UMHP 섬유 10g 오븐 건조 (OD)를 추가한다. <ol><li> 80 ° C 탈 이온수 160 mL를 첨가하여 가수 분해를 종료하기 전에 60 분의 소정의 반응 시간의 끝에서, 산 가수 분해 (약 2 ㎖)의 분취 량을 취. </li></ol></li><li> 설탕 샘플링 분해물 0.5 mL로 희석하고, 산 농도 분석. 15 결정화가 실온으로 옹알 옹알 동안 일어나는의 남은 가수 분해물 샘플을 관찰한다. </li><li> 흐너 깔때기에 여과지를 사용하는 진공 여과에 의해 가수 분해 된 펄프의 가수 분해물을 분리한다. 주 : 이러한 분리는 온도가 강하하기 전에 다소 빠르게 발생해야하고, 산 할지나 용액에서 결정화한다. 때문에 산성 용액에서 높은 이온 세기 때문에, CNC의 생성 가수 분해에 덩어리와는 FCSR 잔차와 함께 머물. 약 산 80 ~ 90 %를 여과로 제거됩니다. </li></ol> 3. CNC 분리 <ol><li> DI 물을 사용하여 섹션 2에서 여과 된 고체를 세척하고 DI 물 약 1 %의 총 고형분에 희석. 10 분 동안 11,960 XG에서 여과 액을 원심 분리기. </li><li> 상층 액을 가만히 따르다. 상등액 혼탁해질 때까지 신선한 DI 물을 사용하여 세척 및 여과 과정을 반복한다. 탁도는 CNC가 분산 콜로이드되기 시작하는 용액의 이온 강도가 충분히 떨어진 것을 나타냅니다. </li><li> 정착 가수 분해 펄프 (2.3)와 혼탁 한 상층 액을 섞는다. 액체의 전도도는 DI 워터의 접근까지 DI 물을 사용하여 투석 백에 혼합물 (14 kDa의 MWCO)를 투석. 컨덕턴스 미터를 사용하여 전도도를 측정. </li><li> 원심 10 분 성상의 CNC 분산액을 얻기위한 3500 XG의 투석 샘플. CNF 생산 즉, 침전 단계, FCSR을 유지합니다. </li><li> 대구 방법을 사용하여 분산액의 CNC의 측정 량으로부터 CNC 수율이 결정은 18 세 이전에 설명했다. </li></ol> 4. CNF 생산 <ol><li> CNC에 분산을 분리 한 후 중량 측정에 의한 침전 FCSR의 수율을 결정합니다. 105 ° C에서 FCSR 건조하여 사용하거나 BEP UMHP 섬유의 초기 오븐 건조 중량에 대하여 FCSR의 오븐 건조 중량을 측정한다. </li><li> 기계적 연속적 모두이 100MPa에서 87 μm의 오리피스 챔버를 통해 2 회이어서 200 ㎛의 오리피스 챔버를 통해 현탁액을 3 회 통과시켜 0.5 %의 섬유 현탁액에 FCSR를 피 브릴. </li></ol> 5. 원자 힘 현미경 (AFM) 이미징 <ol><li> 초음파 처리 약 0.01 중량 % CNC 또는 CNF의2 분 동안 uspensions. 운모 기판 상에 분산 된 현탁액의 방울을 증착. 상온에서 증착 된 현탁액을 공기 - 건조. </li><li> 제조 업체의 프로토콜을 사용하여 모드를 눌러 진동의 공기 건조 CNC는과 CNFs의 AFM 이미지를 가져 가라. 직경 및 길이 분포를 얻기 위해 상용 소프트웨어를 사용하여 약 100 개인 CNC는 또는 CNFs의 AFM 이미지를 분석합니다. </li></ol> 6. 푸리에 유추 (FTIR) 측정을 변환 <ol><li> 에스테르 그룹을 식별하기 위해 원래의 BEP와 UMHP 섬유와 함께 생성 된 CNC 및 CNF 샘플을 분석하는 범용 - 감쇠 전반사 (ATR) 프로브 상업적 FTIR 분광계를 사용한다. </li><li> 450 사이의 파장 범위에서 샘플의 흡수 스펙트럼을 녹음 - 4,000cm -1 4cm -1 각 샘플 4 스캔 해상도. </li></ol> 7. 전도율 적정 <ol><li> ...로서 할 전도율 적정를 사용하여샘플들의 그룹의 내용이 디카 르 복실 산에 의해 에스테르 화에 기인 카르복실기를 ntify. </li><li> 120 mL의 1 mM의 NaCl 용액에 CNC는 또는 CNFs의 50 mg의 (OD)와 CNC 또는 CNF 정지를 추가합니다. 30 초 간격으로 2 mM의 NaOH 용액을 약 0.2 mL를 첨가하여 혼합물을 적정한다. </li><li> 컨덕턴스 미터를 사용하여 전도도를 측정한다. 수산화 나트륨을 첨가하는 과정에서 도전성 곡선의 변곡점 (최저점)을 찾는다. </li><li> C는 NaOH 용액 (몰 / L)의 농도 인 다음의 방정식을 사용하여 변곡점에 소비 된 NaOH 상대 기반으로 카르복실기 (밀리몰 / L)의 양을 계산 V는 (ML 첨가 NaOH 용액의 부피이고 )는 m) OD 무게 (g에서 CNC는 또는 CNFs의 질량이다. <img alt="방정식" src="/files/ftp_upload/55079/55079eq1.jpg" /></li></ol> 8. CNC 및 CNF 열 안정성 결정 <ol><li> t의 열 분해 측정을 수행그는 CNC 및 CNF 열 중량 분석 (TGA)에 의해 샘플. </li><li> 불필요한 산화 분해를 방지하기 위해 20 ㎖ / 분으로 고순도 질소 기류를 사용한 노 퍼지. 시험 전 4 시간 동안 50 ° C에서 샘플을 건조. 건조 중량으로 5 mg의 샘플 크기를 사용한다. </li><li> 노 온도는 10 ℃ / 분의 가열 속도로 대기에서 600 ℃로 증가함에 따라 샘플의 중량을 기록한다. </li><li> 초기 중량 측정 감량 정규화. </li><li> 105 ° C의 오븐에서 CNC와 CNF 샘플들의 개별 열 안정성 테스트를 수행. 종래 그래피하여 (4) 24 시간 후, 샘플의 색의 변화를 기록한다. </li></ol> 9. X-ray 회절 <ol><li> 를 눌러 전술 한 바와 같이 펠렛을 180 MPa의에서 CNC 또는 CNF 샘플을 동결 건조. 38-10의 2θ 범위에서 X 선 회절에서의 Cu-Kα 방사선을 사용하여 펠릿 5 실시 광각 X 선 회절 측정0.02 °의 단계 °. </li><li> 시걸 방법 (19)을 사용하여 펠릿의 결정화도 지수 (CRI)를 계산 (베이스 라인 감산없이). </li></ol>

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첸 주홍은 CNC 및 CNF 생산을위한 디카 르 복실 산을 사용하여 미국 특허 출원의 공동 발명자이다.

전술 한 바와 같이 말레 산 가수 분해로부터 CNC 샘플 두꺼운 CNC 직경은 긴 길이에도 불구하고, 각각 BEP 및 UMHP로부터위한 CNC는 적당한 평균 종횡비가 7.24와 8.53, 결과. CNFs는 각 CNC는보다 긴 길이와 각각 BEP 및 UMHP로부터 CNC는 13.9 및 19.0의 큰 종횡비 결과 얇은 직경, 둘 이상이 있었다. 매우 낮고, 본 연구에서는 미세 유동화에 사용되는 압력 등의 종횡비를 향상시키기 위해 CNF 직경을 감소시키는 심?...

지속 가능한 경제 발전은 재생 및 생분해 성 원료를 사용하지 않을 경우에만 필요하지만 이러한 재생 가능한 원료에서 바이오 및 생화학의 다양한 생산하는 녹색 및 환경 친화적 인 제조 기술을 사용합니다. 이러한 재생 리그 노 셀룰로오스로부터 생성 된 나노 결정 셀룰로오스 (CNC) 셀룰로오스 nanofibrils (CNF)와 같은 셀룰로오스 나노 물질은 생분해 성이며, 바이오 1, 2의 범위를 개발하기에 적합한 고유의 기계적 및 광학적 특성을 갖는다. 순수한 기계적 세동 또는 비 - 재생 또는 처리 화학 불충분 재활용으로 인한 환경 지속 사용시 불행히도 셀룰로오스 나노 물질을 제조하는 기존의 기술은 에너지 중 같은 농축 무기산 가수 분해 공정을 3-8 또는 산화 방법 9-를 사용하는 경우로서 집약적 11. 또한, 산화 방법은 환경 적으로 독성 콤포넌트를 생성 할 수있다리그 노 셀룰로오스와 반응하여 unds. 리그 노 셀룰로오스 - 따라서, 셀룰로오스 나노 물질을 생산하는 녹색 제조 기술을 개발하는 것은 풍부하고 재생 가능 물질의 전체를 사용하기 위해 매우 중요합니다. 헤미셀룰로오스와 셀룰로오스를 용해 해중합하는 산 가수 분해를 사용하여 셀룰로오스 나노 물질을 제조하는 효과적인 접근 방법이다. 고체 산 산 회수 (12, 13)를 용이하게하는 장점과 셀룰로오스 설탕 제조에 사용되어왔다. 진한 무기산을 이용하여 이전의 연구는 낮은 산 농도가 CNC 수율 결정화도 3,5- 개선 된 것으로 나타났다. 이 온화한 산 가수 분해가 CNF (3), (14)와 통합 생산 및 CNC의 접근 방식을 통해 속성과 셀룰로오스 나노 물질의 수율을 향상시킬 수 있습니다 동안 강산은 셀룰로오스의 결정에 손상을 줄 수 있음을 시사한다. 여기에서 우리는 생산은 농축 고체 디카 르 복실 산 가수 분해를 사용하는 방법을 문서화CNF (15)과 함께 전자 CNC. 이러한 디카 르 복실 산 또는 낮은 주위 온도에서 낮은 용해도를 가지며, 따라서 이들은 쉽게 성숙한 결정화 기술을 통해 회수 될 수있다. 또한 비등 또는 압력 용기를 사용하지 않고, 농축 산 가수 분해를 용이하게 승온에서 우수한 용해도를 갖는다. 이들 아미노산은 또한 CNC의 제조에 사용되는 통상적 인 무기산 좋은 CNC의 결정에서의 용도 결과보다 높은 pKa를하고 있으므로, 및 인해 나머지 하부 CNC의 섬유상 셀룰로오스 고체 잔류 상당한 양의 수율 (FCSR 또는 부분 가수 분해 섬유) 불구 불완전 셀룰로오스 해중합. FCSR 낮은 에너지 입력을 사용하여 후속 기계적 세동 통해 CNF의 제조에 사용될 수있다. 무기산을 사용하는 것에 비해 따라서, 당 셀룰로스 손실은 최소화된다. 이곳은 카르복시산이 Speier는 피셔 에스테르 화 (16)를 셀룰로오스 에스테르 화 수 있다고 알려져. 디카 르 복실 산을 적용하면, 반 산 취소 가교 에스테르 (17) (또는 카르 복 실화)가 발생할 수 있습니다 셀룰로오스하는 우리가 이전에 15 입증 된 바와 같이 카르 CNC 및 CNF를 생성 할 수 있습니다. 여기에 설명 된 방법은 생산할 수있는 카르 열적으로 안정한 비교적 간단하고 높은 화학적 복원을 가지는 낮은 에너지 입력을 사용하면서 또한 표백 또는 표백 펄프 중 하나에서 높은 결정 성 CNF와 CNC.

<table><tbody><tr><td>Bleached eucalypus pulp&amp;nbsp;</td><td>Aracruz Cellulose</td><td></td><td></td></tr><tr><td>Unbleached mixed hardwood kraft pulp&amp;nbsp;</td><td>International Paper&amp;nbsp;</td><td></td><td></td></tr><tr><td>Maleic acid</td><td>Sigma-Aldrich</td><td>M0375-1KG/CAS110-16-7</td><td>Powder; assay: 99.0% (HPLC)</td></tr><tr><td>Glycerol</td><td>Sigma-Aldrich</td><td>G5516-4L/CAS56-81-5</td><td></td></tr><tr><td>Sodium hydroxide</td><td>Fisher Scientific</td><td>S318-500/CAS1310-73-2, 497-19-8</td><td>Certified ACS</td></tr><tr><td>Sodium chloride</td><td>Mallinckrodt</td><td>7581-12/CAS7647-14-5</td><td>Crystal,AR</td></tr><tr><td>Cupriethylenediamine solution</td><td>GFS Chemicals</td><td>E32103-1L/CAS14552-35-3</td><td>1 M, for determination of solution viscosity of pulps</td></tr><tr><td>Acetone</td><td>Fisher Scientific</td><td>A18-500/CAS67-64-1</td><td>Certified ACS</td></tr><tr><td>Accu-Test&lt;sup&gt;TM&lt;/sup&gt; Vials for COD Testing</td><td>Bioscience,Inc.</td><td>01-215-28</td><td>COD testing for 20 to 900&amp;nbsp;mg/L standard range concentration</td></tr><tr><td>Heating plate</td><td>IKA</td><td></td><td>Mode: C-MAD HS7 digital</td></tr><tr><td>Magnetic stir bar</td><td>ACE Glass</td><td></td><td></td></tr><tr><td>Pyrex three-neck round-bottom flask</td><td>Sigma-Aldrich</td><td>CLS4965B500-1EA</td><td></td></tr><tr><td>Dialysis tubing cellulose membrane</td><td>Sigma-Aldrich</td><td>D9402-100FT</td><td>Typical molecular weight cut-off = 14,000 kDa</td></tr><tr><td>Disposable aluminum dishes</td><td>Sigma-Aldrich</td><td>Z154857-1PAK</td><td>Circles, 60 mm</td></tr><tr><td>Disintegrator</td><td>Testing Machines Inc.(TMI)</td><td></td><td></td></tr><tr><td>Microfluidizer</td><td>Microfluidics Corporation</td><td></td><td></td></tr><tr><td>Sonicator</td><td>Qsonica LLC.</td><td></td><td>Mode: 3510R-MT, 50-60&amp;nbsp;Hz, 180&amp;nbsp;W</td></tr><tr><td>Zeta potential analyzer</td><td>Brookhaven Instruments Corporation</td><td></td><td></td></tr><tr><td>FTIR</td><td>PerkinElmer</td><td></td><td></td></tr><tr><td>Conductometric titrator</td><td>Yellow Springs Instrument (YSI)</td><td></td><td></td></tr><tr><td>TGA analyzer</td><td>PerkinElmer</td><td></td><td></td></tr><tr><td>X-ray diffractometer</td><td>Bruker Corporation</td><td></td><td></td></tr><tr><td>AFM imging&amp;nbsp;</td><td>AFM Workshop</td><td></td><td></td></tr><tr><td>SEM imaging</td><td>Carl Zeiss</td><td></td><td></td></tr></tbody></table>

green and low-cost production of thermally stable and carboxylated cellulose nanocrystals and nanofibrils using highly recyclable dicarboxylic acids

여기에서 우리는 잠재적으로 낮은 비용과 높은 재활용 디카 르 복실 고체 산을 사용하여 표백 유칼립투스 펄프 (BEP) 및 표백 혼합 나무 크라프트 펄프 (UMHP) 섬유에서 높은 열 안정성 및 카르 셀룰로오스 나노 결정 (CNC는) 및 nanofibrils (CNF)의 녹색 생산을 보여줍니다. 각각 BEP 및 UMHP 들어, 60 분, 120 분, 120 ℃ (상압에서의 비점 없음) 100 ℃에서 70 중량 % - 전형적인 작동 조건 (50)의 산 농도였다. 0.4 밀리몰 / g - 생성 CNC는 0.2에서 해당 피드 섬유보다 높은 열 분해 온도 및 카복실산 기 함량을 갖는다. CNC는 미네랄 산을 사용하여 제조 된 것보다 336 nm의 높은 결정화도 - 낮은 강도 (1.0의 높은 pKa가 - 3.0) 유기산으로는 약 239 이상 길이 모두 CNC는 결과. 설탕에 셀룰로오스 손실을 최소화했다. 디카 르 복실 산 가수 분해 섬유소 고체 잔류 물 (FCSR)을 사용했다낮은 에너지 입력을 후속 기계 세동을 통해 카르 CNFs를 생산하고 있습니다.

피드 산 가수 분해 섬유 대응 SEM 이미지와 함께 BEP 및 UMHP에서 CNC와 CNF의 대표적인 AFM 화상은도 1 및도 2에 나타내었다. 이미지는 분명 (2B와도 1b와도 1a를 비교하고, 2A) 최소 섬유 직경의 변화와 산 가수 분해에 의해, 섬유 길이의 실질적인 감소를 나타낸다. 단축 된 섬유 길이는 또한 섬유의 가수 분해 중합 측...

Watch this Scientific Journal Video about Green and Low-cost Production of Thermally Stable and Carboxylated Cellulose Nanocrystals and Nanofibrils Using Highly Recyclable Dicarboxylic Acids at JoVE.c

Green and Low-cost Production of Thermally Stable and Carboxylated Cellulose Nanocrystals and Nanofibrils Using Highly Recyclable Dicarboxylic Acids

여기에서 우리는 재활용도가 높은 고체 디카 르 복실 산을 사용하여 높은 열 안정성 및 카르 셀룰로오스 나노 결정 (CNC)와 nanofibrils (CNF)의 녹색과 지속 가능한 생산을위한 새로운 방법을 보여줍니다.

열 안정성 및 카르 셀룰로오스 나노 결정과 Nanofibrils를 사용하여 재활용도가 높은 디카 르 복실 산의 녹색과 저비용 생산

Here we demonstrate potentially low cost and green productions of high thermally stable and carboxylated cellulose nanocrystals (CNCs) and nanofibrils ...

green-low-cost-production-thermally-stable-carboxylated-cellulose

Universidad de Cartagena UDEC

Research

JoVE Journal

Chemistry

11.8K 조회수.  Nanjing Forestry University.  여기에서 우리는 재활용도가 높은 고체 디카 르 복실 산을 사용하여 높은 열 안정성 및 카르 셀룰로오스 나노 결정 (CNC)와 nanofibrils (CNF)의 녹색과 지속 가능한 생산을위한 새로운 방법을 보여줍니다. 

비디오: Green and Low-cost Production of Thermally Stable and Carboxylated Cellulose Nanocrystals and Nanofibrils Using Highly Recyclable Dicarboxylic Acids

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and lignin. Layer-by-layer (LbL) assembly process which relies on the assembly of oppositely charged molecules from aqueous solutions was used to build a freestanding composite film of isolated wood polymers of lignin and oxidized nanofibril cellulose (NFC). To facilitate the assembly of these negatively charged polymers, a positively charged polyelectrolyte, poly(diallyldimethylammomium chloride) (PDDA), was used as a linking layer to create this simplified model cell wall. The layered adsorption process was studied quantitatively using quartz crystal microbalance with dissipation monitoring (QCM-D) and ellipsometry. The results showed that layer mass/thickness per adsorbed layer increased as a function of total number of layers. The surface coverage of the adsorbed layers was studied with atomic force microscopy (AFM). Complete coverage of the surface with lignin in all the deposition cycles was found for the system, however, surface coverage by NFC increased with the number of layers. The adsorption process was carried out for 250 cycles (500 bilayers) on a cellulose acetate (CA) substrate. Transparent free-standing LBL assembled nanocomposite films were obtained when the CA substrate was later dissolved in acetone. Scanning electron microscopy (SEM) of the fractured cross-sections showed a lamellar structure, and the thickness per adsorption cycle (PDDA-Lignin-PDDA-NC) was estimated to be 17 nm for two different lignin types used in the study. The data indicates a film with highly controlled architecture where nanocellulose and lignin are spatially deposited on the nanoscale (a polymer-polymer nanocomposites), similar to what is observed in the native cell wall.

The objective of this research was to form synthetic plant cell wall tissue using layer-by-layer assembly of nanocellulose fibrils and isolated lignin assembled from dilute aqueous suspensions.&#160; Surface measurement techniques of quartz crystal microbalance and atomic force microscopy were used to monitor the formation of the polymer-polymer nanocomposite material.

Nanocellulose, 리그닌의 날조 된 자립형 필름, 및 합성 폴리 양이온 : Biomimicking 나무를 향하여

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

연구

화학

Pretreatment of Lignocellulosic Biomass with Low-cost Ionic Liquids

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of a variety of lignocellulosic feedstocks. Here we demonstrate the use of these low-cost protic ILs in the deconstruction of lignocellulosic biomass (Ionosolv pretreatment), yielding cellulose and a purified lignin. In the most generic process, the protic ionic liquid is synthesized by accurate combination of aqueous acid and amine base. The water content is adjusted subsequently. For the delignification, the biomass is placed into a vessel with IL solution at elevated temperatures to dissolve the lignin and hemicellulose, leaving a cellulose-rich pulp ready for saccharification (hydrolysis to fermentable sugars). The lignin is later precipitated from the IL by the addition of water and recovered as a solid. The removal of the added water regenerates the ionic liquid, which can be reused multiple times. This protocol is useful to investigate the significant potential of protic ILs for use in commercial biomass pretreatment/lignin fractionation for producing biofuels or renewable chemicals and materials.

The pretreatment of lignocellulosic biomass with protic low-cost ionic liquids is shown, resulting in a delignified cellulose-rich pulp and a purified lignin. The pulp gives rise to high glucose yields after enzymatic saccharification.

저가 이온 성 액체와 리그 노 셀룰로오스 바이오 매스의 전처리

A number of ionic liquids (ILs) with economically attractive production costs have recently received growing interest as media for the delignification of ...

환경과학

Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While metal-based nanoparticles are associated with synthetic and environmental hassles, cellulose introduces a green, sustainable alternative for nanoparticle synthesis. Here, we present the chemical synthesis and separation procedures to produce new classes of hairy nanoparticles (bearing both amorphous and crystalline regions) and biopolymers based on wood fibers. Through periodate oxidation of soft wood pulp, the glucose ring of cellulose is opened at the C2-C3 bond to form 2,3-dialdehyde groups. Further heating of the partially oxidized fibers (e.g., T = 80 &#176;C) results in three products, namely fibrous oxidized cellulose, sterically stabilized nanocrystalline cellulose (SNCC), and dissolved dialdehyde modified cellulose (DAMC), which are well separated by intermittent centrifugation and co-solvent addition. The partially oxidized fibers (without heating) were used as a highly reactive intermediate to react with chlorite for converting almost all aldehyde to carboxyl groups. Co-solvent precipitation and centrifugation resulted in electrosterically stabilized nanocrystalline cellulose (ENCC) and dicarboxylated cellulose (DCC). The aldehyde content of SNCC and consequently surface charge of ENCC (carboxyl content) were precisely controlled by controlling the periodate oxidation reaction time, resulting in highly stable nanoparticles bearing more than 7 mmol functional groups per gram of nanoparticles (e.g., as compared to conventional NCC bearing &#60;&#60; 1 mmol functional group/g). Atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) attested to the rod-like morphology. Conductometric titration, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), dynamic light scattering (DLS), electrokinetic-sonic-amplitude (ESA) and acoustic attenuation spectroscopy shed light on the superior properties of these nanomaterials.

Synthesis schemes to prepare highly stable wood fiber-based hairy nanoparticles and functional cellulose-based biopolymers have been detailed.

매우 안정, 기능 털이 나노 입자와 목재 섬유에서 생체 고분자 : 지속 가능한 나노 기술쪽으로

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While ...

Manufacturing Of Robust Natural Fiber Preforms Utilizing Bacterial Cellulose as Binder

A novel method of manufacturing rigid and robust natural fiber preforms is presented here. This method is based on a papermaking process, whereby loose and short sisal fibers are dispersed into a water suspension containing bacterial cellulose. The fiber and nanocellulose suspension is then filtered (using vacuum or gravity) and the wet filter cake pressed to squeeze out any excess water, followed by a drying step. This will result in the hornification of the bacterial cellulose network, holding the loose natural fibers together.
Our method is specially suited for the manufacturing of rigid and robust preforms of hydrophilic fibers. The porous and hydrophilic nature of such fibers results in significant water uptake, drawing in the bacterial cellulose dispersed in the suspension. The bacterial cellulose will then be filtered against the surface of these fibers, forming a bacterial cellulose coating. When the loose fiber-bacterial cellulose suspension is filtered and dried, the adjacent bacterial cellulose forms a network and hornified to hold the otherwise loose fibers together.
The introduction of bacterial cellulose into the preform resulted in a significant increase of the mechanical properties of the fiber preforms. This can be attributed to the high stiffness and strength of the bacterial cellulose network. With this preform, renewable high performance hierarchical composites can also be manufactured by using conventional composite production methods, such as resin film infusion (RFI) or resin transfer molding (RTM). Here, we also describe the manufacturing of renewable hierarchical composites using double bag vacuum assisted resin infusion.

We present a novel method of manufacturing rigid and robust short natural fiber preforms using a papermaking process. Bacterial cellulose acts simultaneously as the binder for the loose fibers and provides rigidity to the fiber preforms. These preforms can be infused with a resin to produce truly green hierarchical composites.

바인더로 박테리아 셀룰로오스를 활용하여 강력한 천연 섬유 프리폼 제조

A novel method of manufacturing rigid and robust natural fiber preforms is presented here. This method is based on a papermaking process, whereby loose ...

생체공학

Estimation of Crystalline Cellulose Content of Plant Biomass using the Updegraff Method

Cellulose is the most abundant polymer on Earth generated by photosynthesis and the main load-bearing component of cell walls. The cell wall plays a significant role in plant growth and development by providing strength, rigidity, rate and direction of cell growth, cell shape maintenance, and protection from biotic and abiotic stressors. The cell wall is primarily composed of cellulose, lignin, hemicellulose and pectin. Recently plant cell walls have been targeted for the second-generation biofuel and bioenergy production. Specifically, the cellulose component of the plant cell wall is used for the production of cellulosic ethanol. Estimation of cellulose content of biomass is critical for fundamental and applied cell wall research. The Updegraff method is simple, robust, and the most widely used method for the estimation of crystalline cellulose content of plant biomass. The alcohol insoluble crude cell wall fraction upon treatment with Updegraff reagent eliminates the hemicellulose and lignin fractions. Later, the Updegraff reagent resistant cellulose fraction is subjected to sulfuric acid treatment to hydrolyze the cellulose homopolymer into monomeric glucose units. A regression line is developed using various concentrations of glucose and used to estimate the amount of the glucose released upon cellulose hydrolysis in the experimental samples. Finally, the cellulose content is estimated based on the amount of glucose monomers by colorimetric anthrone assay.

The Updegraff method is the most widely used method for the cellulose estimation. The main purpose of this demonstration is to provide a detailed Updegraff protocol for estimation of cellulose content in plant biomass samples.

Updegraff 방법을 사용하여 식물 바이오매스의 크리스탈 셀룰로오스 함량 추정

Cellulose is the most abundant polymer on Earth generated by photosynthesis and the main load-bearing component of cell walls. The cell wall plays a ...

Synthesis Method for Cellulose Nanofiber Biotemplated Palladium Composite Aerogels

Here, a method to synthesize cellulose nanofiber biotemplated palladium composite aerogels is presented. Noble metal aerogel synthesis methods often result in fragile aerogels with poor shape control. The use of carboxymethylated cellulose nanofibers (CNFs) to form a covalently bonded hydrogel allows for the reduction of metal ions such as palladium on the CNFs with control over both nanostructure and macroscopic aerogel monolith shape after supercritical drying. Crosslinking the carboxymethylated cellulose nanofibers is achieved using 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) in the presence of ethylenediamine. The CNF hydrogels maintain their shape throughout synthesis steps including covalent crosslinking, equilibration with precursor ions, metal reduction with high concentration reducing agent, rinsing in water, ethanol solvent exchange, and CO2 supercritical drying. Varying the precursor palladium ion concentration allows for control over the metal content in the final aerogel composite through a direct ion chemical reduction rather than relying on the relatively slow coalescence of pre-formed nanoparticles used in other sol-gel techniques. With diffusion as the basis to introduce and remove chemical species into and out of the hydrogel, this method is suitable for smaller bulk geometries and thin films. Characterization of the cellulose nanofiber-palladium composite aerogels with scanning electron microscopy, X-ray diffractometry, thermal gravimetric analysis, nitrogen gas adsorption, electrochemical impedance spectroscopy, and cyclic voltammetry indicates a high surface area, metallized palladium porous structure.

A synthesis method for cellulose nanofiber biotemplated palladium composite aerogels is presented.The resulting composite aerogel materials offer potential for catalysis, sensing, and hydrogen gas storage applications.

셀룰로오스 나노 섬유 바이오 템플릿 팔라듐 복합 에어로겔에 대한 합성 방법

Here, a method to synthesize cellulose nanofiber biotemplated palladium composite aerogels is presented. Noble metal aerogel synthesis methods often ...

Fractionation of Lignocellulosic Biomass using the OrganoCat Process

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of raw materials and energy. For these novel and sustainable biorefinery concepts, it is important to use catalysts and solvents that are aligned with the principles of Green Chemistry. Therefore, the implementation of biogenic alternatives can be a promising solution. The lignocellulose pretreatment and fractionation process presented herein-OrganoCat-is an integrated fractionation of lignocellulose into its main components using biogenic acids such as 2,5-furandicarboxylic acid as catalyst. Hemicelluloses and other non-cellulosic polysaccharides are selectively depolymerized by the diluted acid and dissolved, while the crystalline cellulose remains in the solid pulp. In the presence of a second organic phase consisting of biogenic 2-methyltetrahydrofuran, disentangled lignin is extracted in situ. The process allows for the efficient fractionation of the three main components-lignin, cellulose, and non-cellulosic sugars. This helps to focus on the quality of the lignin, the improvement of enzymatic hydrolysis of the cellulose-enriched pulp, and the mild non-cellulosic sugar extraction with low degradation.

OrganoCat is a method for the pretreatment and fractionation of lignocellulose under mild conditions into lignin, fermentable sugars, and cellulose pulp. In a biogenic, biphasic solvent system of water and 2-methyltetrahydrofuran with 2,5-furancarboxylic acid as catalyst, the OrganoCat products are separated in situ for straightforward product recovery.

오가노캣 공정을 이용한 리뇨셀룰로오스 바이오매스의 분획

The shift from a petroleum-based to a more sustainable and bio-based economy requires the development of new refinery concepts to maintain the supply of ...

Bacterial Cellulose Spheres that Encapsulate Solid Materials

Bacterial cellulose (BC) spheres have been increasingly researched since the popularization of BC as a novel material. This protocol presents an affordable and simple method for BC sphere production. In addition to producing these spheres, an encapsulation method for solid particles has also been identified. To produce BC spheres, water, black tea, sugar, vinegar, and bacterial culture are combined in a baffled flask and the contents are agitated. After determining the proper culture conditions for BC sphere formation, their ability to encapsulate solid particles was tested using biochar, polymer beads, and mine waste. Spheres were characterized using ImageJ software and thermal gravimetric analysis (TGA). Results indicate that spheres with 7.5 mm diameters can be made in 7 days. Adding various particles increases the average size range of the BC capsules. The spheres encapsulated 10 - 20% of their dry mass. This method shows low-cost sphere production and encapsulation that is possible with easily obtainable materials. BC spheres may be used in the future as a contaminant removal aid, controlled release fertilizer coating, or soil amendment.

This protocol presents an easy, inexpensive method of forming bacterial cellulose (BC) spheres. This biomaterial can function as an encapsulation medium for solid materials, including biochar, polymer spheres, and mine waste.

고체 물질을 캡슐화하는 세균성 셀룰로오스 구체

Bacterial cellulose (BC) spheres have been increasingly researched since the popularization of BC as a novel material. This protocol presents an ...

공학

Designed for Molecular Recycling: A Lignin-Derived Semi-aromatic Biobased Polymer

The development of chemically recyclable biopolymers offers opportunities within the pursuit of a circular economy. Chemically recyclable biopolymers make a positive effort to solve the issue of polymer materials in the disposal phase after the use phase. In this paper, the production of biobased semi-aromatic polyesters, which can be extracted entirely from biomass such as lignin, is described and visualized. The polymer poly-S described in this paper has thermal properties similar to certain commonly used plastics, such as PET. We developed a Green Knoevenagel reaction, which can efficiently produce monomers from aromatic aldehydes and malonic acid. This reaction has been proven to be scalable and has a remarkably low calculated E-factor. These polyesters with ligno-phytochemicals as a starting point show an efficient molecular recycling with minimal losses. The polyester poly(dihydrosinapinic acid) (poly-S) is presented as an example of these semi-aromatic polyesters, and the polymerization, depolymerization, and re-polymerization are described.

An example of a closed-loop approach towards a circular materials economy is described here. A whole sustainable cycle is presented where biobased semi-aromatic polyesters are designed by polymerization, depolymerization, and then re-polymerized with only slight changes in their yields or final properties.

분자 재활용을 위해 설계: 리닌 유래 반 방향족 생물 기반 폴리머

The development of chemically recyclable biopolymers offers opportunities within the pursuit of a circular economy. Chemically recyclable biopolymers make ...

바이오플라보노이드 방출을 위한 리그닌 마이크로/서브미크론 입자 합성

Green Synthesis, Characterization, Encapsulation, and Measurement of the Release Potential of Novel Alkali Lignin Micro-/Submicron Particles

The applicability of biopolymer micro-/nano- technology in human, veterinary medicine, pharmaceutical, and food technology is rapidly growing due to the great potential of biopolymer-based particles as effective carrier systems. The use of lignin as a basic heteropolymer biomatrix for the design of innovative micro-/submicron formulations allows the achievement of increased biocompatibility and offers various active functional groups presenting opportunities for customization of the physicochemical properties and bioactivities of the formulations for diverse applications. The aim of the present study was to develop a simple and ecofriendly methodology for the synthesis of lignin particles with micro- and submicron size; to evaluate their physicochemical, spectral, and structural characteristics; and to examine their capacity for encapsulation of biologically active molecules and potential for in vitro release of bioflavonoids in simulated gastrointestinal media. The presented methodologies apply cheap and green solvents; easy, straightforward, quick, and sensitive processes requiring little equipment, non-toxic substances, and simple methods for their characterization, the determination of encapsulation capacity towards the poorly water-soluble bioactive compounds morin and quercetin, and the in vitro release potential of the lignin matrices.

저자 스포트라이트: 바이오플라보노이드 전달 향상을 위한 친환경 리그닌 기반 미세입자의 개발 및 특성 분석

We describe novel, simple methodologies of synthesis and characterization of biocompatible lignin micro- and submicron particles. These formulations provide a facile approach for the utilization of the heteropolymer, as well as an alternative for the rational design of multifunctional carrier matrices with potential applicability in biomedicine, pharmaceutical technology, and the food industry.

Green Synthesis, Characterization, Encapsulation, and Measurement of the Release Potential of Novel Alkali Lignin Micro-/Submicron Particles(새로운 알칼리 리그닌 마이크로/서브미크론 입자의 방출 가능성 측정)

The applicability of biopolymer micro-/nano- technology in human, veterinary medicine, pharmaceutical, and food technology is rapidly growing due to the ...