JP2021523250A - 低価値で無駄な脂肪、油、およびグリースをグレードアップするための方法 - Google Patents
低価値で無駄な脂肪、油、およびグリースをグレードアップするための方法 Download PDFInfo
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- JP2021523250A JP2021523250A JP2020560997A JP2020560997A JP2021523250A JP 2021523250 A JP2021523250 A JP 2021523250A JP 2020560997 A JP2020560997 A JP 2020560997A JP 2020560997 A JP2020560997 A JP 2020560997A JP 2021523250 A JP2021523250 A JP 2021523250A
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- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
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Abstract
【選択図】図1
Description
本出願は、2018年5月2日に出願された米国仮特許出願第62/665,991号の利益および優先権を主張し、その内容が、参照によってその全体において本明細書に組み込まれる。
本技術は、一般に、水素化処理のための生物再生可能なフィードストックとして使用され得る組成物の処理に関する。より具体的には、限定するものではないが、本技術は、沈降物、硫黄、窒素、塩素、ポリマー、リン、および全金属の量が低減された処理生成物を生成するための低価値および無駄な脂肪、油、およびグリース組成物をグレードアップするための方法を提供する。
一態様では、組成物を苛性溶液と接触させて、苛性処理された組成物を生成することと、苛性処理された組成物をシリカ粒子と組み合わせて、スラリーを生成することと、スラリーからシリカ粒子を除去して、処理された組成物を生成することと、を含む方法が提供される。組成物は、動物性脂肪、動物性油、植物性脂肪、植物性油、野菜脂肪、野菜油、グリース、使用済み食用油、またはそれらの任意の2つ以上の組み合わせを含む。さらに、組成物は、少なくとも約10wppmの全金属、少なくとも約8wppmのリン、少なくとも約10wppmの塩素、少なくとも約10wppmの硫黄、少なくとも約20wppmの窒素、少なくとも約5重量%の遊離脂肪酸を含み、かつ約10〜約150mgKOH/gの酸価を有する。シリカ粒子は、約10ミクロン〜約50ミクロンの平均粒子サイズおよび約200m2/g〜約1000m2/gのブルナウアー−エメット−テラー表面積(「BET表面積」)を有する。
以下、様々な実施形態について記載する。具体的な実施形態は、包括的な説明として、または本明細書で考察される、より広い態様への限定として意図されないことに留意されたい。特定の実施形態に関連して記載された1つの態様は、その実施形態に必ずしも限定されず、任意の他の実施形態で実施することができる。
化石燃料をバイオ燃料に置き換えることで、バイオ燃料の生産に使用されるフィードストックに依存する温室効果ガスの排出が削減する。ほとんどの野菜油と異なり、低価値で無駄な脂肪、油、およびグリース(「FOG」)は、食品加工産業や水処理プラントからの非食用副産物や廃棄物の流れである。例えば、再生可能なディーゼルの生産では、脂質フィード(様々な遊離脂肪酸(「FFA」)含有量を有する)が水素化処理反応器でイソパラフィン系炭化水素に変換される。水素化処理反応器は、典型的には、水素化金属(例えば、Ni、Mo、Co、W、Pd、およびPt)を含浸させた触媒押出物が充填された高圧容器である。
使用済み食用油(UCO)および非食用トウモロコシ油(ICO)を含む未加工FOGブレンドを、硫黄、窒素、および塩素化合物について分析した。表2は、未加工FOGに含まれる硫黄、窒素、塩素の量をまとめたものである。
(a)試験後、全塩素測定の前に試料を水洗すると、塩素の値が60%以上低下することが確認された。
(b)酸価は、滴定によって測定され、2で割って%FFAを得た。
表3に示すブレンド成分および量を使用して、低価値の未加工FOGフィードストックのブレンドを調製した。
(表3)
使用済み食用油および高級で漂白可能な獣脂を含む未加工FOGストリームをICP分析にかけた(表6)。未加工FOGストリームを約2%(重量酸/重量FOG)の割合でクエン酸水溶液と混合し、直列に配置された3つのディスクスタック遠心分離機で遠心分離した。蒸気凝縮液は、遠心分離機の洗浄水として使用された。水は、第3の遠心分離機に入り、その中の重相は第2の遠心分離機に入り、そこから第1の遠心分離機に入り、それによって第1、第2、および第3の遠心分離機を通って流れるFOG/軽相に向流する。苛性溶液(水中25%NaOH)は、第2の遠心分離機に入る重相と混合された。苛性溶液の流量は、第3の遠心分離機からの重相が4〜4.5のpHを有するように制御された。
未加工FOGに含まれる様々な非食用獣脂およびイエローグリースは、溶解ポリエチレン(PE)のAOCS技術Ca16−75に従ってポリマー含有量について測定された。未加工FOG組成物は、標準的な金網フィルタで濾過された。PEの結果は、検出値以下から11,000ppm(1.1重量%)までの範囲であった。混合FOG組成物フィードをクエン酸で処理し、実施例1の条件に従って遠心分離した。第3の遠心分離機からの軽相は、数日間の操作で定期的に採取され、溶解PEのAOCS法に従ってポリマーを試験した。様々な試料のPE結果は、50〜80ppmの範囲であり、脱ガム工程だけでは溶解ポリマーが除去されなかったことを示す。
本技術の方法は、様々な低価値のFOG組成物フィードブレンドについて経時的に評価された。性能は、未加工フィードの酸価の関数としてのリンおよび金属の低減率として測定された。驚くべきことに、図1および2で観察されたように、20mgKOH/g(10%FFA)未満のFOG酸価は、図1および2の白丸で示されているように、本技術の方法による処理後、リンおよび全金属の最大95%の低減を示した(実施例1)。しかしながら、20mgKOH/g(図1および2の黒丸で示されている)を超える値については、酸価の増加に伴う性能の低減が観察された。
高アルカリ度を特徴とする未加工FOGフィードストックは、アルカリ度を低減し、余分な金属を除去するために、前処理工程(preconditioning step)で処理された。この連続的な前処理プロセスでは、ブラウングリースの流れは、質量ベースで5%のブラウングリースの割合で飽和蒸気と混合され、約80℃に加熱した。蒸気注入の直後に、市販の50%クエン酸水溶液をブラウングリース質量ベースで1重量%の割合で添加した。酸処理は、石鹸を中和し、金属イオンをキレート化する目的を有した。平均滞留時間が30〜60分の混合容器は、混合物を均質化し、クエン酸の完全な分散と接触を確保するために使用された。酸性化した水および油の混合物は、混合タンクから3相遠心分離機にポンプで送られ、不溶性の塩および不純物をスラッジとして除去した。3相遠心分離機は、オージェリング作用によって2つの液相から固体を機械的に抽出するスクロール部材の実装を通じて、固体および沈殿物の連続的な除去を提供した。3相遠心分離機は、軽い油相の一部も重相とともに除去されるように微調整され、それによって重相のほぼ完全な除去が保証された。水溶性の塩、金属、およびその他の水溶性不純物は、重い水相の一部として除去された。軽い油相は、ボトムスフラクションベースで95%を超える収率で回収された。前処理プロセス全体での油の総アルカリ度および不純物の低減を表8に示す。
組成物を苛性溶液と接触させて、苛性処理された組成物を生成する工程と、
苛性処理された組成物をシリカ粒子と組み合わせて、スラリーを生成する工程と、
スラリーからシリカ粒子を除去して、処理された組成物を生成する工程と
を含む方法であって、
組成物が、
動物性脂肪、動物性油、植物性脂肪、植物性油、野菜脂肪、野菜油、グリース、および使用済み食用油のうちの1つ以上と、
少なくとも約10wppmの全金属と、
少なくとも約8wppmのリンと、
少なくとも約10wppmの塩素と、
少なくとも約10wppmの硫黄と、
少なくとも約20wppmの窒素と、
少なくとも約5重量%の遊離脂肪酸と
を含み、かつ
約10mgKOH/g〜約150mgKOH/gの酸価を有し、
シリカ粒子が、約10ミクロン〜約50ミクロンの平均粒子サイズおよび約200m2/g〜約1000m2/gのBET表面積を有する、方法。
B.組成物が、動物性脂肪、動物性油、植物性脂肪、植物性油、野菜脂肪、野菜油、グリース、またはそれらの任意の2つ以上の混合物を含む、パラグラフAの方法。
C.組成物が、イエローグリース、ブラウングリース、浮遊グリース、家禽脂肪、非食用トウモロコシ油、使用済み食用油、非食用獣脂、浮遊獣脂、パームスラッジ油、またはそれらの任意の2つ以上の混合物を含む、パラグラフAまたはパラグラフBの方法。
D.全金属が、As、Ca、Cr、Cu、Fe、K、Li、Mg、Mn、Na、Ni、Pb、Sr、およびZnからなる群から選択される1つ以上のメンバーを含む、パラグラフA〜Cのいずれか1つに記載の方法。
E.組成物が、約0.05wppm〜約11,000wppmのポリマーをさらに含む、パラグラフA〜Dのいずれか1つに記載の方法。
F.組成物が、約10mgKOH/g〜約50mgKOH/gの酸価を有する、パラグラフA〜Eのいずれか1つに記載の方法。
G.組成物が、約10mgKOH/g〜約30mgKOH/gの酸価を有する、パラグラフA〜Fのいずれか1つに記載の方法。
H.組成物が、約5重量%〜約15重量%の遊離脂肪酸を含む、パラグラフA〜Gのいずれか1つに記載の方法。
I.組成物を苛性溶液と接触させる前に、組成物がグリセロール分解プロセスを受けて、組成物中に約5重量%〜約15重量%の遊離脂肪酸を提供する、パラグラフA〜Hのいずれか1つに記載の方法。
J.組成物を苛性溶液と接触させる前に、酸脱ガム工程をさらに含む、パラグラフA〜Iのいずれか1つに記載の方法。
K.組成物を苛性溶液と接触させる前に、アルカリ度低減工程をさらに含む、パラグラフA〜Jのいずれか1つに記載の方法。
L.組成物を漂白粘土と接触させる工程を含まない、パラグラフA〜Kのいずれか1つに記載の方法。
M.苛性溶液が、水酸化アンモニウム水溶液、水酸化カリウム水溶液、水酸化ナトリウム水溶液、またはそれらの任意の2つ以上の組み合わせを含む、パラグラフA〜Lのいずれか1つに記載の方法。
N.シリカ粒子が、アモルファスシリカ粒子を含む、パラグラフA〜Mのいずれか1つに記載の方法。
O.シリカ粒子が、苛性処理された組成物の重量に対するシリカ粒子の重量に基づいて約0.1%(w/w)〜約0.8%(w/w)で苛性処理された組成物と組み合わされる、パラグラフA〜Nのいずれか1つに記載の方法。
P.シリカ粒子が、約2.0〜約6.0の水溶液pHを有する、パラグラフA〜Oのいずれか1つに記載の方法。
Q.シリカ粒子との組み合わせが、約150°F〜約200°Fの温度で行われ、スラリーが、約100トルから約500トルの絶対圧力に供される、パラグラフA〜Pのいずれか1つに記載の方法。
R.シリカ粒子との組み合わせが、連続流操作タンク内で行われる、パラグラフA〜Qのいずれか1つに記載の方法。
S.シリカ粒子との組み合わせが、約10分から約90分の滞留時間を含む、パラグラフA〜Rのいずれか1つに記載の方法。
T.方法が、スラリーを珪藻土(DE)と組み合わせる工程をさらに含み、DE対シリカ粒子の重量比が約0.1:1〜約1.5:1である、パラグラフA〜Sのいずれか1つに記載の方法。
U.除去が、1つ以上のフィルタでスラリーを濾過することを含む、パラグラフA〜Tのいずれか1つに記載の方法。
V.1つ以上のフィルタが、圧力リーフフィルタを含み、圧力リーフフィルタが、任意選択で、DE、セルロース、およびパーライトのうちの少なくとも1つ以上でプレコートされている、請求項Uに記載の方法。
W.処理された組成物が、
少なくとも約5重量%〜約10重量%の遊離脂肪酸と、
約10wppm未満の全金属と、
約5wppm未満のリンと、
約5wppm未満の塩素と、
約5wppm未満の硫黄と、
約100wppm未満の窒素と
を含み、かつ
10mgKOH/g〜約20mgKOH/gの酸価を有する、パラグラフA〜Vのいずれか1つに記載の方法。
X.方法が、処理された組成物を水素化処理する工程をさらに含む、パラグラフA〜Wのいずれか1つに記載の方法。
Claims (24)
- 組成物を苛性溶液と接触させて、苛性処理された組成物を生成する工程と、
前記苛性処理された組成物をシリカ粒子と組み合わせて、スラリーを生成する工程と、
前記スラリーから前記シリカ粒子を除去して、処理された組成物を生成する工程と
を含む方法であって、
前記組成物が、
動物性脂肪、動物性油、植物性脂肪、植物性油、野菜脂肪、野菜油、グリース、および使用済み食用油のうちの1つ以上と、
少なくとも約10wppmの全金属と、
少なくとも約8wppmのリンと、
少なくとも約10wppmの塩素と、
少なくとも約10wppmの硫黄と、
少なくとも約20wppmの窒素と、
少なくとも約5重量%の遊離脂肪酸と
を含み、かつ
約10mgKOH/g〜約150mgKOH/gの酸価を有し、
前記シリカ粒子が、約10ミクロン〜約50ミクロンの平均粒子サイズおよび約200m2/g〜約1000m2/gのBET表面積を有する、方法。 - 前記組成物が、動物性脂肪、動物性油、植物性脂肪、植物性油、野菜脂肪、野菜油、グリース、またはそれらの任意の2つ以上の混合物を含む、請求項1に記載の方法。
- 前記組成物が、イエローグリース、ブラウングリース、浮遊グリース、家禽脂肪、非食用トウモロコシ油、使用済み食用油、非食用獣脂、浮遊獣脂、パームスラッジ油、またはそれらの任意の2つ以上の混合物を含む、請求項1に記載の方法。
- 前記全金属が、As、Ca、Cr、Cu、Fe、K、Li、Mg、Mn、Na、Ni、Pb、Sr、およびZnからなる群から選択される1つ以上のメンバーを含む、請求項1に記載の方法。
- 前記組成物が、0wppm〜約11,000wppmのポリマーをさらに含む、請求項1に記載の方法。
- 前記組成物が、約10mgKOH/g〜約50mgKOH/gの酸価を有する、請求項1に記載の方法。
- 前記組成物が、約10mgKOH/g〜約30mgKOH/gの酸価を有する、請求項1に記載の方法。
- 前記組成物が、約5重量%〜約15重量%の遊離脂肪酸を含む、請求項1に記載の方法。
- 前記組成物を前記苛性溶液と接触させる前に、前記組成物がグリセロール分解プロセスを受けて、前記組成物中に約5重量%〜約15重量%の遊離脂肪酸を提供する、請求項1に記載の方法。
- 前記組成物を苛性溶液と接触させる前に、酸脱ガム工程をさらに含む、請求項1に記載の方法。
- 前記組成物を苛性溶液と接触させる前に、アルカリ度低減工程をさらに含む、請求項1に記載の方法。
- 前記組成物を漂白粘土と接触させる工程を含まない、請求項1に記載の方法。
- 前記苛性溶液が、水酸化アンモニウム水溶液、水酸化カリウム水溶液、水酸化ナトリウム水溶液、またはそれらの任意の2つ以上の組み合わせを含む、請求項1に記載の方法。
- 前記シリカ粒子が、アモルファスシリカ粒子を含む、請求項1に記載の方法。
- 前記シリカ粒子が、前記苛性処理された組成物の重量に対する前記シリカ粒子の重量に基づいて約0.1%(w/w)〜約0.8%(w/w)で前記苛性処理された組成物と組み合わされる、請求項1に記載の方法。
- 前記シリカ粒子が、約2.0〜約6.0の水溶液pHを有する、請求項1に記載の方法。
- 前記シリカ粒子との前記組み合わせが、約150°F〜約200°Fの温度で行われ、前記スラリーが、約100トル〜約500トルの絶対圧力に供される、請求項1に記載の方法。
- 前記シリカ粒子との前記組み合わせが、連続流操作タンク内で行われる、請求項1に記載の方法。
- 前記シリカ粒子との前記組み合わせが、約10分〜約90分の滞留時間を含む、請求項1に記載の方法。
- 前記方法が、前記スラリーを珪藻土(DE)と組み合わせる工程をさらに含み、DE対シリカ粒子の重量比が約0.1:1〜約1.5:1である、請求項1に記載の方法。
- 前記除去が、1つ以上のフィルタで前記スラリーを濾過することを含む、請求項1に記載の方法。
- 前記1つ以上のフィルタが、圧力リーフフィルタを含み、前記圧力リーフフィルタが、任意選択で、DE、セルロース、およびパーライトのうちの少なくとも1つ以上でプレコートされている、請求項21に記載の方法。
- 前記処理された組成物が、
少なくとも約5重量%〜約10重量%の遊離脂肪酸と、
約10wppm未満の全金属と、
約5wppm未満のリンと、
約5wppm未満の塩素と、
約5wppm未満の硫黄と、
約100wppm未満の窒素と
を含み、かつ
10mgKOH/g〜約20mgKOH/gの酸価を有する、
請求項1〜22のいずれか一項に記載の方法。 - 前記処理された組成物を水素化処理する工程をさらに含む、請求項1〜23のいずれか一項に記載の方法。
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JPS6327600A (ja) * | 1986-05-14 | 1988-02-05 | ダブリユー・アール・グレイス・アンド・カンパニー−コネチカツト | グリセリド油の精製方法 |
JPH02150495A (ja) * | 1988-05-06 | 1990-06-08 | W R Grace & Co | グリセリド油の二相吸着及び処理 |
JPH07216380A (ja) * | 1991-04-03 | 1995-08-15 | Wr Grace & Co Connecticut | グリセリド油、脂肪化学薬品及びワツクスエステル処理のためのmpr法 |
US20050081436A1 (en) * | 2003-10-09 | 2005-04-21 | Bryan Bertram | Purification of biodiesel with adsorbent materials |
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US5336794A (en) * | 1986-05-14 | 1994-08-09 | W. R. Grace & Co.-Conn. | Dual phase adsorption and treatment of glyceride oils |
US5231201A (en) * | 1986-05-14 | 1993-07-27 | W. R. Grace & Co.-Conn. | Modified caustic refining of glyceride oils for removal of soaps and phospholipids |
US5252762A (en) * | 1991-04-03 | 1993-10-12 | W. R. Grace & Co.-Conn. | Use of base-treated inorganic porous adsorbents for removal of contaminants |
US6248911B1 (en) * | 1998-08-14 | 2001-06-19 | Pq Corporation | Process and composition for refining oils using metal-substituted silica xerogels |
US6822105B1 (en) | 2003-08-12 | 2004-11-23 | Stepan Company | Method of making alkyl esters using glycerin |
US7803343B2 (en) * | 2007-06-27 | 2010-09-28 | J.M. Huber Corporation | Silica gel manufacturing method and gels made thereby |
SG11201507576WA (en) | 2013-03-14 | 2015-10-29 | Reg Synthetic Fuels Llc | Method of removing a contaminant from a contaminant-containing biological composition useful as a biofuel feedstock |
HUE049020T2 (hu) | 2013-06-11 | 2020-08-28 | Renewable Energy Group Inc | Eljárás biodízel és az abból nyert termékek elõállítására |
UY35649A (es) * | 2013-07-09 | 2015-02-27 | Reg Seneca Llc | ?producción de productos a partir de materias primas que contienen ácidos grasos libres?. |
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JPS6327600A (ja) * | 1986-05-14 | 1988-02-05 | ダブリユー・アール・グレイス・アンド・カンパニー−コネチカツト | グリセリド油の精製方法 |
JPH02150495A (ja) * | 1988-05-06 | 1990-06-08 | W R Grace & Co | グリセリド油の二相吸着及び処理 |
JPH07216380A (ja) * | 1991-04-03 | 1995-08-15 | Wr Grace & Co Connecticut | グリセリド油、脂肪化学薬品及びワツクスエステル処理のためのmpr法 |
US20050081436A1 (en) * | 2003-10-09 | 2005-04-21 | Bryan Bertram | Purification of biodiesel with adsorbent materials |
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BR112020022313A2 (pt) | 2021-05-18 |
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WO2019213157A1 (en) | 2019-11-07 |
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CN112469806A (zh) | 2021-03-09 |
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UY38209A (es) | 2019-11-29 |
US20210371771A1 (en) | 2021-12-02 |
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US20230303948A1 (en) | 2023-09-28 |
KR20210002682A (ko) | 2021-01-08 |
SG11202010794SA (en) | 2020-11-27 |
EP3788124A1 (en) | 2021-03-10 |
US11118133B2 (en) | 2021-09-14 |
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