JP5967730B2 - リグノセルロース系バイオマスからのリグニンの製造 - Google Patents
リグノセルロース系バイオマスからのリグニンの製造 Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31971—Of carbohydrate
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- Y10T428/31978—Cellulosic next to another cellulosic
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Description
本出願は、その開示内容全体が参照により本明細書に組み込まれる、2011年5月4日出願の米国特許出願第61/482,479号明細書の利益を主張する。
第1圧力および第1温度でリグノセルロース系バイオマスを提供する工程であって、前記リグノセルロース系バイオマスが:
不溶性リグニン;
を含む第1固体画分;
可溶性C6サッカリド;
可溶性リグニン;
を含む第1液体画分;
を含む、工程と、
前記第1圧力下にて、前記リグノセルロース系バイオマスの前記第1温度を、リグニンのガラス転移温度を少なくとも約1℃超える第2温度に下げる工程と、
前記第2温度での前記リグノセルロース系バイオマスの前記第1圧力を、約1秒未満の時間で第2圧力に下げ、前記第1液体画分中の前記可溶性リグニンを沈殿させ、かつ
不溶性リグニン;
沈殿リグニン;
を含む第2固体画分;
可溶性C6サッカリド;
を含む第2液体体画;
を含む混合物が形成される工程と、
を含む、リグノセルロース系バイオマスからリグニンを製造する方法であって、
前記不溶性リグニンおよび沈殿リグニンの平均粒径が約500ミクロン未満である、方法に関する。
約500ミクロン以下の平均サイズを有するリグニンを含む組成物であって、
前記リグニンが、超臨界流体抽出または近臨界流体抽出を用いて、リグノセルロース系バイオマスから処理される、組成物に関する。
第1圧力および第1温度でリグノセルロース系バイオマスを提供する工程であって、前記リグノセルロース系バイオマスが:
不溶性リグニン;
を含む第1固体画分;
可溶性C6サッカリド;
可溶性リグニン;
を含む第1液体画分;
を含む、工程と、
前記第1圧力下にて、前記リグノセルロース系バイオマスの前記第1温度を、リグニンのガラス転移温度を少なくとも約1℃超える第2温度に下げる工程と、
前記第2温度での前記リグノセルロース系バイオマスの前記第1圧力を、約1秒未満の時間で第2圧力に下げ、前記第1液体画分中の前記可溶性リグニンを沈殿させ、かつ
不溶性リグニン;
沈殿リグニン;
を含む第2固体画分;
可溶性C6サッカリド;
を含む第2液体画分;
を含む混合物が形成される工程と、
を含む、リグノセルロース系バイオマスからリグニンを製造する方法であって、
前記不溶性リグニンおよび沈殿リグニンの平均粒径が約500ミクロン未満である、方法に関する。
臨界流体抽出または近臨界流体抽出を用いてリグノセルロース系バイオマスから処理されるリグニン;
を含む組成物に関する。
前処理(分画)およびセルロース加水分解プロセスによって、供給原料として使用されるリグノセルロース系バイオマスからリグニンが遊離される。この実施例における試験のために、セルロース流出液のフラッシングから生成されたリグニン試料を試験し、発熱量、近似、最終、および灰溶融温度、灰酸化物組成、含水率および粒径を決定した。
重力および20μm濾紙を利用して、フラッシュされたセルロース加水分解流出液グルコースストリームから、リグニンが分離される場合、リグニンは平均含水率65〜75重量%を有する。これはさらに、遠心機または真空濾過ユニットを使用して低減され、母液から固形分をさらに効果的に分離することができる。代表的なリグニン試料は、グルコース生成物タンクの底で回収されるスラッジから得られ、その生成物は、約225バールおよび375℃のセルロース加水分解条件にて100メッシュ木粉の複数回の実施から生成された。続いて、この試料を空気乾燥させて、その乾燥率を測定した。
種々の含水率のリグニンの発熱量を分析した。燃料の発熱量は、酸素によるその完全な燃焼中に放出される熱の尺度である。いずれの燃料も水素を含有し、水素が空気中で燃焼すると、燃焼生成物として水が形成される。この生成された水は蒸気状態を維持することができるか、あるいは凝縮することができて液体を形成し、相変化に伴う気化潜熱のために測定発熱量の実質的な違いが生じる。燃料ユニットによって放出される熱を決定する場合には、発生した水がすべて凝縮され、したがって、発熱量が気化潜熱を組み込む場合に想定されるよりも、より高位の(または総)発熱量(HHV)が通常報告される。より低位の(または正味)発熱量(LHV)については、水が全く凝縮していないと想定されており、燃焼生成物のすべてが気体状態を維持する。HHVは、酸素燃焼式熱量計を使用して決定することができ、燃料の単位重量当たりに関する熱(Btu/ポンドf)によって表される。LHVの決定は、以下の等式から計算され得る:
HHV=LHV+nHvp
式中:
HHV=燃料高位発熱量(Btu/ポンドf)
LHV=燃料高位発熱量(Btu/ポンドf)
n=消費された燃料の質量当たりの、発生した水の理論質量(ポンドw/ポンドf)
Hvp=水の気化潜熱(Btu/ポンドw)
個々の粒子の表面積/質量比は、燃焼効率、ボイラーのデザイン、および燃焼空気の導入方法に影響することから、燃料としてのリグニンの有用性の重要な側面である。適切に分粒されていない燃料は完全に燃焼できず、炭素豊富なボトムアッシュおよび/またはフライアッシュの形で熱エネルギーが失われ得る。粒径の測定は、分級、例えば篩い分けによって、または顕微鏡下にて代表的な試料を観察し、適切なスケールと比較することによって行われ得る。Magnaview DC5−153顕微鏡および較正スケーリングスライドを用いて、平均粒径が決定された。セルロース加水分解から誘導された分離固形物に関して、確認された平均粒子直径は含水率37%で10〜30μmであり、その固形分はおよそリグニン80%であると決定された。
燃料の近似分析から、揮発物、固定炭素、含水率、および燃料中に存在する灰が乾燥燃料重量のパーセンテージとして示される。揮発物と固定炭素のパーセンテージのどちらも、燃料の発熱量、火炎温度、および燃焼プロセスに一般に直接的な影響を有する。炭素および金属以外、他のすべての燃料が気体として燃焼する。揮発物のパーセンテージは、気相中で燃焼するであろう燃料の量を表し、残存する炭素は火格子上で固体として、または微粒子として燃焼する。灰含有率は、大気汚染制御装置、ボイラーの火格子、およびボトムアッシュ処理装置の設計において重要である。
燃料の最終分析から、燃料試料の乾燥重量のパーセンテージとしてその元素組成が示される。一般に考慮される主要な元素は、炭素(C)、水素(H)、窒素(N)、硫黄(S)、および酸素(O)であり、元素ではないが、灰である。大気汚染制御装置の効果的な設計において、かつ大気排出許可(air permitting)において使用される、二酸化硫黄(SOx)および粒状物質(PM)の空気放出率を正確に推定するのに必要であることから、硫黄および灰のパーセンテージは特に重要である。
灰の溶融温度は、還元性雰囲気および酸化性雰囲気の両方において、高温炉内の観察窓を通して燃料(リグニン)の灰を盛り上げた試料を見ることによって決定される。円錐、角錐、または立方体形の灰を1000℃を超えて着実に加熱し、可能な限り高い温度、好ましくは1600℃(2910°F)に加熱する。次いで、以下の温度が記録される:
・初期変形温度(IT):マウンドのポイントが最初に変形し、丸くなり始めた時に達成される。
・軟化(球形)温度(ST):これは、マウンドの頂部が球形となった時、つまり円錐の底面、がその高さに等しい時に達成される。
・半球形温度(HT):これは、マウンド全体が半球形となった時、つまり円錐の底面がその高さの2倍である時に達成される。
・流動(流体)温度(FT):これは、溶融灰が炉の床に崩壊して平らなボタンが形成される時、つまり広がって一体化した塊となった時に達成される。
一般に、還元下の温度は、酸化条件下の相当する温度以下である。これらの温度の差は一般に、灰の鉄含有率が増加するにしたがって増加する。溶融温度は、IT、ST、HT、およびFTの順序で単調に増加するはずである。
灰の酸化鉱物組成は、リグニンの燃焼によって生成される灰がバイオマスボイラーの燃焼チャンバ内でいかに挙動するかを理解するのにも有用である。組成、特に鉄レベルおよび塩基対酸酸化物の比は、溶融温度の範囲に影響する。一般的な分析から、以下の酸化鉱物、シリカ(SiO2)、アルミナ(Al2O3)、酸化第二鉄(Fe2O3)、二酸化チタン(TiO2)、五酸化リン(P2O5)、酸化カルシウム(CaO)、酸化マグネシウム(MgO)、酸化マンガン(MnO)、酸化ナトリウム(Na2O)、酸化カリウム(K2O)、および三酸化硫黄(SO3)の重量パーセンテージが決定される。シリカ、アルミナ、および二酸化チタンは、塩基性酸化物を形成する残りの化合物と酸性酸化物の群を構成する。
Claims (15)
- リグノセルロース系バイオマスを加水分解により糖化リグノセルロース系バイオマスが生じる第1圧力および第1温度にする工程であって、前記リグノセルロース系バイオマスが:
不溶性リグニン;
を含む第1固体画分;
可溶性C6サッカリド;
可溶性リグニン;
を含む第1液体画分;
を含む、工程と、
前記第1圧力下にて、前記リグノセルロース系バイオマスの前記第1温度を、リグニンのガラス転移温度を少なくとも1℃超える第2温度に下げる工程と、
前記第2温度での前記リグノセルロース系バイオマスの前記第1圧力を、1秒未満の時間で、リグニンがそのガラス転移温度を下回る温度となる、第2圧力に下げ、前記第1液体画分中の前記可溶性リグニンを沈殿させ、かつ
不溶性リグニン;
沈殿リグニン;
を含む第2固体画分;
可溶性C6サッカリド;
を含む第2液体画分;
を含む混合物が形成される工程と、
を含むことを特徴とする、リグノセルロース系バイオマスからリグニンを製造する方法。 - 請求項1に記載の方法において、連続的であることを特徴とする、方法。
- 請求項1に記載の方法において、前記混合物の温度を下げることをさらに含むことを特徴とする、方法。
- 請求項1に記載の方法において、重力によって、前記不溶性リグニンおよび前記沈殿リグニンを分離させることをさらに含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記第2固体画分と前記第2液体画分を分離することをさらに含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記第2圧力が気圧を超えることを特徴とする、方法。
- 請求項6に記載の方法において、前記第2圧力を気圧に下げることをさらに含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記第2圧力が気圧であることを特徴とする、方法。
- 請求項1に記載の方法において、少なくとも1つの熱交換器を使用して、熱を回収することをさらに含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記提供工程前に、前記リグノセルロース系バイオマスを分画して、C5サッカリドの少なくとも一部を除去することを特徴とする、方法。
- 請求項10に記載の方法において、前記分画する工程は、熱水処理を含むことを特徴とする、方法。
- 請求項11に記載の方法において、前記熱水処理は、圧縮熱水、亜臨界水、近臨界水、または超臨界水を含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記不溶性リグニンおよび沈殿リグニンの平均粒径が500ミクロン未満であることを特徴とする、方法。
- 請求項1に記載の方法において、前記第1液体画分が水を含むことを特徴とする、方法。
- 請求項1に記載の方法において、前記第1温度は280℃から375℃であることを特徴とする、方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201161482479P | 2011-05-04 | 2011-05-04 | |
US61/482,479 | 2011-05-04 | ||
PCT/US2012/036591 WO2012151524A2 (en) | 2011-05-04 | 2012-05-04 | Lignin production from lignocellulosic biomass |
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JP2014516090A JP2014516090A (ja) | 2014-07-07 |
JP2014516090A5 JP2014516090A5 (ja) | 2015-06-25 |
JP5967730B2 true JP5967730B2 (ja) | 2016-08-10 |
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JP2014509493A Active JP5967730B2 (ja) | 2011-05-04 | 2012-05-04 | リグノセルロース系バイオマスからのリグニンの製造 |
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US (2) | US8663800B2 (ja) |
EP (1) | EP2705111A4 (ja) |
JP (1) | JP5967730B2 (ja) |
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WO2012151524A2 (en) | 2012-11-08 |
CN103502383B (zh) | 2016-06-08 |
US8840995B2 (en) | 2014-09-23 |
ZA201309032B (en) | 2015-03-25 |
EP2705111A2 (en) | 2014-03-12 |
KR20140039215A (ko) | 2014-04-01 |
EP2705111A4 (en) | 2014-11-19 |
AU2012250575B2 (en) | 2015-03-26 |
CA2806873C (en) | 2014-07-15 |
US20140030524A1 (en) | 2014-01-30 |
BR112013028149A2 (pt) | 2017-04-25 |
RU2012154206A (ru) | 2014-06-20 |
CA2806873A1 (en) | 2012-11-08 |
JP2014516090A (ja) | 2014-07-07 |
WO2012151524A3 (en) | 2013-03-21 |
SG194724A1 (en) | 2013-12-30 |
RU2602068C2 (ru) | 2016-11-10 |
AU2012250575A1 (en) | 2013-11-07 |
NZ616832A (en) | 2015-11-27 |
MY171010A (en) | 2019-09-23 |
CN103502383A (zh) | 2014-01-08 |
US8663800B2 (en) | 2014-03-04 |
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