木質纖維原料之木質素提取之方法Method for extracting lignin from lignocellulosic material
本發明係有關於一種木質纖維原料之木質素提取之方法，尤指涉及一種兩階段木質素提取方法，特別係指製程可達到高純度之木質素高提取量，能避免木質素析出顆粒過小，且節省用水，有效降低蒸發濃縮與乾燥溫度，達到節能之效果者。The invention relates to a method for extracting lignin of a lignocellulosic material, in particular to a method for extracting a two-stage lignin, in particular to a high extraction amount of lignin which can achieve high purity, and can prevent lignin precipitation particles from being too small. And save water, effectively reduce the evaporation concentration and drying temperature, to achieve the effect of energy saving.
經由溶劑前處理方式所提取出之木質素（Lignin），由於該種木質素僅溶於溶劑中，當溶劑揮發或是在液體轉移存放容器時，木質素很容易黏附在存放之器皿上，造成木質素提取之困難。對此，遂有下列各項處理提取方式之提出。 按，美國專利US 8227004號，係藉由調節pH值，然後用水快速稀釋將木質素沉澱；惟本發明不需調整pH值，透過使用物理性蒸發乾燥及溶劑稀釋，即可達到木質素之沉澱析出。美國專利US 9303127號，係使用乳酸代替乙醇從木質纖維素生物質中提取木質素，在約55°C狀態下，透過加入過量的水可提取11倍的木質素；惟本發明操作溫度低，且無需耗費大量用水。台灣專利201715100/I575124號，係揭露使用一種甘油-氯化膽鹼深共熔溶劑處理纖維原料之方法將木質素分離 ，於高溫下可有82.13%之木質素回收率；惟本發明所提製程無需使用特殊共熔劑，亦無需在高溫下操作。 另有Guo, Y等人所提文獻一（Guo, Y., Zhou J., Wen J., Sun, G., and Sun, Y., 2015. Structural transformations of triploid of Populus tomentosa Carr. lignin during auto-catalyzed ethanol organosolv pretreatment. Industrial Crops and Products. 76(15):522-529.），該文獻於反應後，水解液在50°C進行減壓濃縮後，再加入3倍體積之純水將木質素沉澱出；惟本發明減壓濃縮操作溫度較低，且濃縮率僅需50%。Yanez-S M等人所提文獻二（Yanez-S M., Matsuhiro B., Nunez C., Pan S., Hubbell CA., Sannigrahi P., and Ragauskas AJ., 2014. Physicochemical characterization of ethanol organosolv lignin (EOL) from Eucalyptus globulus: Effect of extraction conditions on the molecular structure. Polymer Degradation and Stability. 110:184-194.），該文獻中木質素係從水解液酸化至pH=2後沉澱析出，之後再用70°C的水洗滌乾燥；惟本發明無須將溶液酸化，而是使用物理性蒸發乾燥及溶劑稀釋，即可達到木質素之沉澱析出。以及Fan, L等人所提文獻三（Fan, L., Ruan, R., Liu, Y., Wang, Y. and Tu, C., 2015. Effects of extraction conditions on the characteristics of ethanol organosolv lignin from bamboo (Phyllostachys pubescens Mazel). BioResources. 10(4):7998-8013.），該文獻於反應後，水解液混合進行減壓濃縮後再加入10倍體積的純水將木質素沉澱析出；惟本發明針對減壓濃縮訂定一套濃縮率之標準，濃縮率僅需50%，且無需耗費大量用水。 由上述各項習知技術可知，若再使用溶劑將黏附之木質素洗下來，溶劑的再次回收將造成成本提高，而有導致整體成本上升之問題。另一處理提取方式則是利用直接加水稀釋，其雖然可以達到木質素提取，但是會耗費大量用水，而木質素析出顆粒太小、不易分離，且溶劑的再次利用率低，造成增加木質素提取之操作成本。 有鑑於木質纖維植物中，纖維素及半纖維素都可以經由解聚及酵素分解後轉為糖類，作為後續之生質能源或生質化學品之應用，但其中之木質素卻沒辦法有效地從木質纖維植物中被分離，即使被分離出來，但也純度不高且分離效果不佳。故，ㄧ般習用者係無法符合使用者於實際使用時達到高純度之木質素高提取量，避免木質素析出顆粒過小 ，且節省用水，降低蒸發濃縮與乾燥溫度，達到節能效果之所需。Lignin extracted by solvent pretreatment, because the lignin is only soluble in the solvent, when the solvent is volatilized or in the liquid transfer storage container, the lignin easily adheres to the storage vessel, resulting in Difficulties in lignin extraction. In this regard, there are the following ways to deal with the extraction method. According to U.S. Patent No. 8,227,004, the lignin is precipitated by adjusting the pH and then rapidly diluting with water; however, the present invention does not require adjustment of the pH value, and the precipitation of lignin can be achieved by using physical evaporative drying and solvent dilution. Precipitate. U.S. Patent No. 9,303,127, which uses lactic acid instead of ethanol to extract lignin from lignocellulosic biomass, and extracts 11 times of lignin by adding excess water at about 55 ° C; however, the operating temperature of the present invention is low. It does not require a lot of water. Taiwan Patent No. 201715100/I575124 discloses the method of separating lignin by using a glycerol-choline choline deep eutectic solvent to treat fiber raw materials, and has a lignin recovery rate of 82.13% at a high temperature; No special eutectics are required and there is no need to operate at high temperatures. Another article by Guo, Y., Zhou J., Wen J., Sun, G., and Sun, Y., 2015. structural transformations of triploid of Populus tomentosa Carr. lignin during auto 76(15):522-529.), after the reaction, the hydrolyzate is concentrated under reduced pressure at 50 ° C, and then 3 times the volume of pure water is added to the wood. The quality precipitated; however, the operating temperature of the reduced pressure concentration of the present invention is low, and the concentration rate is only 50%. Yanez-S M., et al. (Yanez-S M., Matsuhiro B., Nunez C., Pan S., Hubbell CA., Sannigrahi P., and Ragauskas AJ., 2014. Physicochemical characterization of ethanol organosolv lignin (EOL) from Eucalyptus globulus: Effect of extraction conditions on the molecular structure. Polymer Degradation and Stability. 110: 184-194.), in which the lignin is precipitated from the hydrolyzate to pH=2, and then used again. The water is washed and dried at 70 ° C; however, the present invention does not need to acidify the solution, but uses physical evaporation drying and solvent dilution to achieve precipitation of lignin. And Fan, L., Ruan, R., Liu, Y., Wang, Y. and Tu, C., 2015. Effects of extraction conditions on the characteristics of ethanol organosolv lignin from Bamboo (Phyllostachys pubescens Mazel). BioResources. 10(4):7998-8013.), after the reaction, the hydrolyzate is mixed and concentrated under reduced pressure, and then 10 times of pure water is added to precipitate lignin; The invention sets a set of concentration rate standards for decompression concentration, which requires only 50% concentration and does not require a large amount of water. It is known from the above-mentioned various techniques that if the adhered lignin is washed away by using a solvent, the re-recycling of the solvent causes an increase in cost, and there is a problem that the overall cost rises. Another treatment extraction method is to use direct water dilution, although it can achieve lignin extraction, but it will consume a lot of water, and the lignin precipitation particles are too small, difficult to separate, and the solvent reuse rate is low, resulting in increased lignin extraction. Operating costs. In view of the fact that in lignocellulosic plants, both cellulose and hemicellulose can be converted into sugars by depolymerization and decomposition of enzymes, which can be used as a subsequent biomass energy or biochemical, but the lignin is not effective. It is isolated from lignocellulosic plants, and even if it is isolated, it is not pure and has a poor separation effect. Therefore, the general users can not meet the high extraction purity of lignin in the user's actual use, avoid lignin precipitation particles too small, and save water, reduce evaporation concentration and drying temperature, to achieve energy-saving effect.
本發明之主要目的係在於，克服習知技藝所遭遇之上述問題並提供一種為提高木質纖維原料之木質素提取，使用較低溫及低壓條件下初步析出較大顆粒木質素，利用加水稀釋濃縮液之溶劑比例，使剩餘之小顆粒木質素析出並黏附在大顆粒木質素上，再經由攪拌混凝達到木質素之高提取率及高純度，不僅能避免木質素析出顆粒過小，且節省用水，可有效降低蒸發濃縮與乾燥溫度，達到節能效果之木質纖維原料之木質素提取之方法。 本發明之次要目的係在於，提供一種製程操作步驟簡易，且不須額外調整酸鹼值步驟或特殊設備操作來進行木質素提取，有利木質素之快速提取，且操作成本低廉有利技術移轉之木質纖維原料之木質素提取之方法。 本發明之另一目的係在於，提供一種可解決單獨使用溶劑蒸發法下，不易將溶劑濃度降至木質素可析出濃度以下，及木質素固著於器壁難以分離等問題之木質纖維原料之木質素提取之方法。 本發明之再一目的係在於，提供一種可解決單獨使用加水稀釋法下，用水過多及木質素顆粒太小難以沉澱析出等問題之木質纖維原料之木質素提取之方法。 為達以上之目的，本發明係一種木質纖維原料之木質素提取之方法，係於木質纖維原料進行酸催化溶劑前處理法分離後，自富含木質素及半纖維素解聚物之液相溶液中以兩階段方式提取高純度木質素，其至少包含下列步驟：（Ａ）蒸發步驟：利用旋轉蒸發裝置，於42～46°C之水浴及蒸發壓力介於130～85 mbar之低壓條件下，將該液相溶液進行蒸發回收溶劑及初步析出較大顆粒木質素；以及（Ｂ）加水稀釋步驟：配合該液相溶液之濃縮率，於剩餘之濃縮液中加入純水稀釋濃縮液，使加水稀釋後之溶劑濃度範圍介於13～16%，配合攪拌混凝使剩餘之小顆粒木質素析出並黏附在大顆粒木質素上，取得高提取率與高純度之木質素，其中於不同濃縮率下，該木質素之提取率皆可達80%以上，純度為93%以上。 於本發明上述實施例中，該酸催化溶劑前處理法係使用單一種醇類溶劑與水添加少量無機酸，與該木質纖維原料以固液比介於5～15%進行木質纖維素組成之解聚分離前處理製程，固液分離後木質素及半纖維素主要存在該液相溶液中，其中該醇類溶劑濃度介於40～70%，該無機酸之酸濃度介於0.5～5.0%。 於本發明上述實施例中，當該蒸發回收溶劑比例達到50～70%時，於該濃縮液中加入純水稀釋濃縮液，進行攪拌8～12小時。 於本發明上述實施例中，該木質素之提取率為88%，純度為97.11%。 於本發明上述實施例中，該木質纖維原料係可選自稻稈、蔗渣、芒草、狼尾草、柳枝稷、玉米稈、木材及竹子。 於本發明上述實施例中，該木質纖維原料係切碎至1～2 cm之物料。The main object of the present invention is to overcome the above problems encountered in the prior art and to provide a method for improving the lignin extraction of lignocellulosic materials, using a relatively low temperature and low pressure condition to preliminarily precipitate larger lignin, and diluting the concentrate with water. The ratio of the solvent causes the remaining small particles of lignin to precipitate and adhere to the large particle lignin, and then achieves high extraction rate and high purity of lignin by stirring and coagulation, thereby not only preventing the lignin precipitation particles from being too small, and saving water, The method for extracting lignin of lignocellulosic material which can effectively reduce evaporation concentration and drying temperature and achieve energy saving effect. The secondary object of the present invention is to provide a process operation step that is simple, and does not require additional adjustment of the pH value step or special equipment operation for lignin extraction, is advantageous for rapid extraction of lignin, and has low operating cost and advantageous technology transfer. A method for extracting lignin from a lignocellulosic material. Another object of the present invention is to provide a lignocellulosic material which can solve the problem that the solvent concentration is not reduced below the lignin precipitation concentration and the lignin is fixed on the wall of the vessel, which is difficult to separate under the solvent evaporation method. The method of lignin extraction. Still another object of the present invention is to provide a method for extracting lignin of a lignocellulosic material which can solve the problems of excessive use of water and lignin particles which are too small to be precipitated and precipitated under the use of a water-diluting method. For the purpose of the above, the present invention relates to a method for extracting lignin from a lignocellulosic material, which is obtained from a liquid phase rich in lignin and hemicellulose depolymerized after separation of the lignocellulosic material by acid-catalyzed solvent pretreatment. The high-purity lignin is extracted in a two-stage manner in the solution, and comprises at least the following steps: (A) evaporation step: using a rotary evaporation apparatus, a water bath at 42 to 46 ° C and a low pressure condition of evaporating pressure of 130 to 85 mbar The liquid phase solution is subjected to evaporation to recover the solvent and preliminarily precipitates the larger particle lignin; and (B) the water dilution step: mixing the concentration ratio of the liquid phase solution, adding the pure water to the remaining concentrated solution to dilute the concentrated liquid, so that The solvent concentration after dilution with water is in the range of 13-16%, and the remaining small particle lignin is precipitated and adhered to the large particle lignin with stirring and coagulation to obtain high extraction rate and high purity lignin, wherein different concentration At the rate, the extraction rate of the lignin can reach more than 80%, and the purity is over 93%. In the above embodiment of the present invention, the acid-catalyzed solvent pretreatment method uses a single alcohol solvent and water to add a small amount of inorganic acid, and the lignocellulosic material is composed of lignocellulose at a solid-liquid ratio of 5 to 15%. Depolymerization pre-treatment process, lignin and hemicellulose are mainly present in the liquid phase solution after solid-liquid separation, wherein the alcohol solvent concentration is 40-70%, and the acid concentration of the mineral acid is 0.5-5.0% . In the above embodiment of the present invention, when the ratio of the evaporation recovery solvent reaches 50 to 70%, the concentrate is diluted with pure water and stirred for 8 to 12 hours. In the above embodiment of the invention, the extraction rate of the lignin is 88% and the purity is 97.11%. In the above embodiment of the present invention, the lignocellulosic material may be selected from the group consisting of rice straw, bagasse, miscanthus, pennisetum, switchgrass, corn stalk, wood, and bamboo. In the above embodiment of the invention, the lignocellulosic material is chopped to a material of 1 to 2 cm.
為了提高木質素之提取，並且希望提取之木質素具高純度，將其具有芳香族化學結構特性，開發應用為苯酚類產品以及碳纖維及其衍生產品等，提高生質原料之利用性。請參閱『第１圖及第２圖』所示，係本發明一具體實施例之木質纖維原料之木質素提取之方法流程示意圖、及本發明製程之不同濃縮率下之木質素提取率示意圖。如圖所示：本發明係一種木質纖維原料之木質素提取之方法，係於木質纖維原料進行酸催化溶劑前處理法分離後，自富含木質素及半纖維素解聚物之液相溶液中提取高純度木質素之一種方法。 由於該種前處理方法所得木質素之特性係可溶解於高溶劑濃度之溶劑與水的混合物中但難溶於水，因此將系統中溶劑濃度降低後，木質素便可團聚成固體進而析出。本發明係採用一種兩階段木質素提取方法，其至少包含下列步驟： 蒸發步驟s11：利用旋轉蒸發裝置，於42～46°C之低溫水浴及蒸發壓力介於130～85 mbar之低壓條件下，將上述液相溶液進行蒸發回收溶劑及初步析出較大顆粒木質素；以及 加水稀釋步驟s12：配合該液相溶液之濃縮率（換言之，當該蒸發回收溶劑比例達到50～70%時），於剩餘之濃縮液中加入純水稀釋濃縮液，使加水稀釋後之溶劑濃度範圍介於13～16%，配合8～12小時攪拌混凝，使剩餘之小顆粒木質素析出並黏附在大顆粒木質素上，取得高提取率與高純度之木質素；經濃縮率測試，本發明從該液相溶液中最高可提取回收81.96%之木質素，此時木質素純度為97.11%；且於不同濃縮率下，該木質素之提取率皆可達80%以上，純度為93%以上。如是，藉由上述揭露之流程構成一全新之木質纖維原料之木質素提取之方法。 上述酸催化溶劑前處理法係將選自稻稈、蔗渣、芒草、狼尾草、柳枝稷、玉米稈、木材及竹子等木質纖維原料，經由切碎機切碎至1～2 cm之適當尺寸後，使用單一種醇類溶劑與水並添加少量催化劑（例如：無機酸）混合，以固液比介於5～15%進行木質纖維素組成之解聚分離前處理製程，固液分離後木質素及半纖維素主要存在該液相溶液中 。其中該醇類溶劑濃度介於40～70%，該無機酸之酸濃度介於0.5～5.0%。 以下係提供利用本發明之實施例以舉例說明本發明之優點與功效： [實施例一] 將822.9g木質素及半纖維素之解聚物溶液加入2000ml濃縮瓶中，以45°C水浴槽加熱濃縮瓶中之溶液，蒸發冷凝管設定7°C，當濃縮瓶液體溫度達到45°C時，初始以130 mbar之壓力開始蒸發溶液，每10分鐘減少10 mbar，最低至85 mbar為止。秤量濃縮瓶中之溶液，當溶液減少至389.3 g時，已達到濃縮率小於50%之目標，則停止蒸發製程，進入第二階段加水稀釋處理，將剩餘濃縮液取出，加入兩倍剩餘濃縮液重之純水（即778.6 g），使用磁石攪拌器以100rpm轉速，將該稀釋溶液進行攪拌混凝持續10小時。混凝析出結束後，使用8 μm孔隙之濾紙進行抽氣過濾，將提取出來之固體從溶液中分離，分離所得木質素固體以45°C進行乾燥，乾燥至恆重（重量變化±0.2mg）後，得到固體物重24.87 g，經組成成分分析，確認得到固體木質素純度為96.73%，木質素從液相中之提取率為80.58%。 [實施例二] 將901.9 g木質素及半纖維素之解聚物溶液加入2000 ml濃縮瓶中，以45°C水浴槽加熱濃縮瓶中之溶液，蒸發冷凝管設定7°C，當濃縮瓶液體溫度達到45°C時，初始以130 mbar之壓力開始蒸發溶液，每10分鐘減少10 mbar，最低至85 mbar為止。秤量濃縮瓶中之溶液，當溶液減少至415.3 g時，已達到濃縮率小於40%之目標，則停止蒸發製程，進入第二階段加水稀釋處理，將剩餘濃縮液取出，加入兩倍剩餘濃縮液重之純水（即930.6 g），使用磁石攪拌器以100rpm轉速，將該稀釋溶液進行攪拌混凝持續10小時。混凝析出結束後，使用8 μm孔隙之濾紙進行抽氣過濾，將提取出來之固體從溶液中分離，分離所得木質素固體以45°C進行乾燥，乾燥至恆重（重量變化±0.2mg）後，得到固體物重27.51 g，經組成成分分析，確認得到固體木質素純度為97.11%，木質素從液相中之提取率為81.96%。 本發明之目的為提高木質纖維原料之木質素提取，使用較低溫及低壓條件下初步析出較大顆粒木質素，利用加水稀釋濃縮液之溶劑比例，使剩餘之小顆粒木質素析出並黏附在大顆粒木質素上，再經由攪拌混凝達到木質素之高提取率及高純度。藉此，本發明之操作步驟簡易，且不須額外調整酸鹼值步驟或特殊設備操作來進行木質素提取，有利木質素之快速提取，且操作成本低廉有利技術移轉。有別於一般習知單獨使用加水稀釋或單獨使用溶劑蒸發之方式，本發明所提方法可解決單獨使用溶劑蒸發法下，不易將溶劑濃度降至木質素可析出濃度以下及木質素固著於器壁難以分離等問題，亦可解決單獨使用加水稀釋法下，用水過多及木質素顆粒太小難以沉澱析出等問題。 綜上所述，本發明係一種木質纖維原料之木質素提取之方法，可有效改善習用之種種缺點，製程之目的為達到高純度之木質素高提取率，不僅能避免木質素析出顆粒過小，且節省用水，可有效降低蒸發濃縮與乾燥溫度，達到節能之效果，進而使本發明之□生能更進步、更實用、更符合使用者之所須，確已符合發明專利申請之要件，爰依法提出專利申請。 惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍；故，凡依本發明申請專利範圍及發明說明書內容所作之簡單的等效變化與修飾，皆應仍屬本發明專利涵蓋之範圍內。In order to improve the extraction of lignin, and to extract the lignin with high purity, it has aromatic chemical structural characteristics, and is developed and applied as a phenol product, carbon fiber and its derivative products, etc., to improve the utilization of raw materials. Referring to FIG. 1 and FIG. 2, it is a schematic diagram of a process for extracting lignin from a lignocellulosic material according to an embodiment of the present invention, and a schematic diagram of lignin extraction rate at different concentration rates of the process of the present invention. As shown in the figure: the present invention is a method for extracting lignin from lignocellulosic material, which is a liquid phase solution rich in lignin and hemicellulose depolymerized after separation of lignocellulosic material by acid-catalyzed solvent pretreatment. A method of extracting high-purity lignin. Since the characteristics of the lignin obtained by this pretreatment method are soluble in a mixture of a solvent and water having a high solvent concentration but are hardly soluble in water, the lignin can be agglomerated into a solid and precipitated after the solvent concentration in the system is lowered. The present invention employs a two-stage lignin extraction method comprising at least the following steps: evaporation step s11: using a rotary evaporation apparatus at a low temperature water bath of 42 to 46 ° C and a low pressure condition of an evaporation pressure of 130 to 85 mbar, The liquid phase solution is subjected to evaporation to recover the solvent and preliminarily precipitates the larger particle lignin; and the water dilution step s12: the concentration ratio of the liquid phase solution is matched (in other words, when the evaporation recovery solvent ratio reaches 50 to 70%), The remaining concentrated liquid is added with pure water to dilute the concentrated liquid, and the solvent concentration after dilution with water is in the range of 13 to 16%, and the mixture is stirred and coagulated for 8 to 12 hours, so that the remaining small particles of lignin are precipitated and adhered to the large granular wood. In terms of quality, high extraction rate and high purity lignin are obtained; according to the concentration rate test, the present invention can extract and extract 81.96% of lignin from the liquid solution, and the purity of lignin is 97.11%; At the rate, the extraction rate of the lignin can reach more than 80%, and the purity is over 93%. As such, a novel method of lignin extraction of lignocellulosic materials is constructed by the above disclosed process. The above acid-catalyzed solvent pretreatment method is selected from the group consisting of straw fiber, bagasse, miscanthus, pennisetum, switchgrass, corn stalk, wood and bamboo, and is chopped to a suitable size of 1 to 2 cm by a chopper. a single alcohol solvent is mixed with water and a small amount of a catalyst (for example, a mineral acid) is mixed, and a solid solution ratio of 5 to 15% is used to carry out a prepolymerization separation pretreatment process of lignocellulose, and lignin after solid-liquid separation And hemicellulose is mainly present in the liquid phase solution. The alcohol solvent concentration is 40 to 70%, and the inorganic acid acid concentration is 0.5 to 5.0%. The following examples are provided to illustrate the advantages and effects of the present invention: [Example 1] 822.9 g of a solution of lignin and hemicellulose depolymerization solution was added to a 2000 ml concentrated bottle at 45 ° C water bath. The solution in the concentrate bottle was heated, and the evaporating condenser was set at 7 ° C. When the concentration of the concentrate bottle reached 45 ° C, the solution was initially evaporated at a pressure of 130 mbar, reducing 10 mbar every 10 minutes, down to 85 mbar. Weigh the solution in the concentrate bottle. When the solution is reduced to 389.3 g, the concentration rate is less than 50%. Stop the evaporation process, enter the second stage and add water to dilute the solution, remove the remaining concentrate, and add twice the remaining concentrate. Heavy pure water (i.e., 778.6 g) was stirred and coagulated at 100 rpm using a magnet stirrer for 10 hours. After the coagulation precipitation was completed, the 8 μm pore filter paper was used for suction filtration, and the extracted solid was separated from the solution, and the separated lignin solid was dried at 45 ° C and dried to constant weight (weight change ± 0.2 mg). Thereafter, a solid matter weight of 24.87 g was obtained, and it was confirmed by compositional analysis that the purity of the solid lignin was 96.73%, and the extraction ratio of lignin from the liquid phase was 80.58%. [Example 2] 901.9 g of lignin and hemicellulose depolymerized solution was added to a 2000 ml concentrated bottle, and the solution in the concentrated bottle was heated in a 45 ° C water bath, and the evaporating condenser was set at 7 ° C. When the liquid temperature reached 45 ° C, the solution was initially started to evaporate at a pressure of 130 mbar, reducing 10 mbar every 10 minutes, down to 85 mbar. Weigh the solution in the concentrate bottle. When the solution is reduced to 415.3 g and the concentration rate is less than 40%, stop the evaporation process, enter the second stage and add water to dilute the treatment, remove the remaining concentrate, and add twice the remaining concentrate. Heavy pure water (i.e., 930.6 g) was stirred and coagulated at 100 rpm using a magnet stirrer for 10 hours. After the coagulation precipitation was completed, the 8 μm pore filter paper was used for suction filtration, and the extracted solid was separated from the solution, and the separated lignin solid was dried at 45 ° C and dried to constant weight (weight change ± 0.2 mg). Thereafter, a solid matter weight of 27.51 g was obtained, and it was confirmed by compositional analysis that the purity of the solid lignin was 97.11%, and the extraction ratio of lignin from the liquid phase was 81.96%. The purpose of the invention is to improve the lignin extraction of the lignocellulosic material, and to preliminarily precipitate the larger granular lignin under the conditions of lower temperature and low pressure, and to dilute the solvent ratio of the concentrated liquid by adding water, so that the remaining small particle lignin is precipitated and adhered to the large On the granular lignin, the high extraction rate and high purity of lignin are achieved by stirring and coagulation. Thereby, the operation steps of the invention are simple, and the lignin extraction is not required to additionally adjust the pH value step or the special equipment operation, and the lignin is quickly extracted, and the operation cost is low, and the technology is transferred. Different from the conventional method of separately using water dilution or solvent evaporation alone, the method of the invention can solve the problem that the solvent concentration is not easily reduced to below the lignin precipitation concentration and the lignin is fixed in the solvent evaporation method alone. The problem that the wall is difficult to separate, etc., can also solve the problem of excessive use of water and lignin particles too small to precipitate and precipitate under the use of the water dilution method alone. In summary, the present invention is a method for extracting lignin from lignocellulosic materials, which can effectively improve various disadvantages of the conventional use. The purpose of the process is to achieve high extraction rate of high-purity lignin, and not only to prevent lignin precipitation particles from being too small, And saving water, can effectively reduce the evaporation concentration and drying temperature, and achieve the effect of energy saving, thereby making the invention of the invention more progressive, more practical, more in line with the needs of the user, and indeed meet the requirements of the invention patent application, File a patent application according to law. However, the above is only the preferred embodiment of the present invention, and the scope of the present invention is not limited thereto; therefore, the simple equivalent changes and modifications made in accordance with the scope of the present invention and the contents of the invention are modified. All should remain within the scope of the invention patent.
s11~s12‧‧‧步驟S11~s12‧‧‧Steps
第１圖，係本發明一具體實施例之木質纖維原料之木質素提取之方 法流程示意圖。 第２圖，係本發明製程之不同濃縮率下之木質素提取率示意圖。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view showing the process flow for lignin extraction of lignocellulosic materials according to an embodiment of the present invention. Fig. 2 is a schematic view showing the lignin extraction rate at different concentration rates of the process of the present invention.