CN115627300A - One-pot method for dismantling three components of lignocellulosic biomass in acidic two-phase system - Google Patents
One-pot method for dismantling three components of lignocellulosic biomass in acidic two-phase system Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
本发明属于生物质化学品制备技术领域，公开了一种酸性两相体系一锅法拆解木质纤维生物质三大组分的方法。包括以下操作步骤：将一定量的酸以及经磨粉抽提后的木质纤维生物质原料加入反应罐中，再加入一定量的水溶液和有机溶液，封装于反应器中升温进行反应，反应后取出反应罐冷却至室温，即可得到富含木糖/阿拉伯糖的水溶液，溶解木质素和含有少量糠醛的有机溶液，以及剩余富含纤维素的固体残渣。本发明方法具有反应过程简单、反应效率高的特点，木糖/阿拉伯糖得率为3.12％‑100.00％，半纤维素脱除率为34.25％‑98.15％，纤维素保留率为72.26％‑97.05％，木质素脱除率为22.59％‑89.37％。
The invention belongs to the technical field of biomass chemical preparation, and discloses a one-pot method for dismantling three major components of lignocellulosic biomass in an acidic two-phase system. It includes the following operation steps: add a certain amount of acid and lignocellulosic biomass raw materials after grinding and extraction into the reaction tank, then add a certain amount of aqueous solution and organic solution, package them in the reactor and heat up for reaction, and take out after the reaction After the reaction tank is cooled to room temperature, an aqueous solution rich in xylose/arabinose, an organic solution containing dissolved lignin and a small amount of furfural, and a solid residue rich in cellulose can be obtained. The method of the invention has the characteristics of simple reaction process and high reaction efficiency, the yield rate of xylose/arabinose is 3.12%-100.00%, the removal rate of hemicellulose is 34.25%-98.15%, and the retention rate of cellulose is 72.26%-97.05% %, the lignin removal rate was 22.59%‑89.37%.
Description
技术领域technical field
本发明属于生物质化学预处理技术领域，具体涉及一种酸性两相体系一锅法高选择性拆解木质纤维生物质三大组分的方法。The invention belongs to the technical field of biomass chemical pretreatment, and in particular relates to a method for dismantling three major components of lignocellulosic biomass with high selectivity in an acidic two-phase system in one pot.
背景技术Background technique
木质纤维生物质预处理拆解三大素可为后续其制备增值化学品如燃料乙醇、γ-戊内酯等的生产提供强有力的技术支持，在强调发展绿色能源的今天具有十分重要的意义。Lignocellulosic biomass pretreatment and disassembly of the three major elements can provide strong technical support for the subsequent production of value-added chemicals such as fuel ethanol, γ-valerolactone, etc., which is of great significance in today's emphasis on the development of green energy .
通常木质纤维生物质预处理只是将三大组分中的一种脱除，如脱除木质素，剩余成分为由半纤维素和纤维素组成的综纤维素；由于半纤维素是三大组分中最易脱除的部分，也会选择性水解去除半纤维素，剩余成分则由纤维素和木质素构成。以上，都不能一步将三大组分有效分离获得，不能分别充分利用生物质的所有组分。Usually lignocellulosic biomass pretreatment only removes one of the three major components, such as lignin removal, and the remaining component is hemicellulose composed of hemicellulose and cellulose; since hemicellulose is one of the three major components The most easily removed part of the fraction is also selectively hydrolyzed to remove hemicellulose, and the remaining components are composed of cellulose and lignin. None of the above can effectively separate and obtain the three major components in one step, and cannot fully utilize all the components of the biomass respectively.
基于两相体系的生物质预处理可有效将木质纤维生物质三大组分分离，又有研究将其称之为Organocat，但此时所用的酸只能是有机酸，包括草酸和呋喃二甲酸；有机相目前只有2-甲基四氢呋喃(2-MeTHF)一种。基于此，目前还没有其他有机酸或无机酸应用于两相体系下的生物质预处理；也没有其他来源于石油化工的其他有机溶剂被应用于该体系作为有机相；更没有两相体系预处理概念的提出。Biomass pretreatment based on a two-phase system can effectively separate the three major components of lignocellulosic biomass, and some studies call it Organocat, but the acids used at this time can only be organic acids, including oxalic acid and furandicarboxylic acid ; The organic phase currently only has 2-methyltetrahydrofuran (2-MeTHF). Based on this, no other organic acid or inorganic acid has been applied to the biomass pretreatment under the two-phase system; no other organic solvents from petrochemical industry have been applied to this system as the organic phase; and there is no two-phase system pretreatment. Handle concept presentation.
目前有文献提出了Organocat预处理(Fractionation of lignocellulosicbiomass using the OrganoCat process,Green Chem.,2015,17,3533)，但其使用的酸仅为草酸，有机溶剂只有2-甲基四氢呋喃一种，且该文献未对比不同溶剂体积比的问题。该文献提供的方法局限性大，反应效果较差。At present, there are literatures that propose Organocat pretreatment (Fractionation of lignocellularbiomass using the OrganoCat process, Green Chem., 2015, 17, 3533), but the acid used is only oxalic acid, and the organic solvent is only 2-methyltetrahydrofuran, and the The literature does not compare the problem of different solvent volume ratios. The method provided by this document has large limitations and poor response effect.
发明内容Contents of the invention
为了弥补现有的木质纤维生物质预处理方法不能一步将生物质三大组分有效拆分并分别分离获得的不足，开发基于两相体系下的一锅法酸水解预处理具有广阔的应用前景。In order to make up for the deficiency that the existing lignocellulosic biomass pretreatment method cannot effectively separate and separate the three major components of biomass in one step, the development of a one-pot acid hydrolysis pretreatment based on a two-phase system has broad application prospects .
本发明的目的在于提供一种两相体系下的一锅法酸水解预处理的方法，实现半纤维素、木质素和纤维素的高选择性拆解及组分定向迁移不同相。The purpose of the present invention is to provide a one-pot acid hydrolysis pretreatment method under a two-phase system, to realize highly selective disassembly of hemicellulose, lignin and cellulose and directional migration of components into different phases.
本发明的目的通过以下技术方案实现。The purpose of the present invention is achieved through the following technical solutions.
一种酸性两相体系一锅法高选择性拆解木质纤维生物质三大组分的方法，包括以下步骤：A method for dismantling the three major components of lignocellulosic biomass with high selectivity by one-pot method in an acidic two-phase system, comprising the following steps:
在反应罐中加入经磨粉抽提后的木质纤维生物质原料、酸，加入有机溶剂和水溶液，反应罐封装在反应器中并升温进行反应，反应结束后的反应罐冷却至室温，即可得到富含木糖/阿拉伯糖的水溶液，富含木质素或者木质素和糠醛的有机溶液，以及富含纤维素的固体残渣。最终产物为黄色或深棕色的分层溶液，固体残渣分散于底部。Add lignocellulosic biomass raw materials and acid after grinding and extraction into the reaction tank, add organic solvent and aqueous solution, the reaction tank is packaged in the reactor and the temperature is raised for reaction, after the reaction is completed, the reaction tank is cooled to room temperature. An aqueous solution rich in xylose/arabinose, an organic solution rich in lignin or lignin and furfural, and a solid residue rich in cellulose are obtained. The final product is a yellow or dark brown layered solution with a solid residue dispersed at the bottom.
优选的，所述木质纤维生物质原料包括麦草秸秆、玉米秸秆、木材、灌木等。Preferably, the lignocellulosic biomass raw material includes wheat straw, corn straw, wood, shrubs and the like.
优选的，所述酸为有机酸或无机酸，其中，有机酸包括对甲苯磺酸、草酸、呋喃二甲酸、L-苹果酸、丙二酸、顺丁烯二酸、酒石酸等，无机酸包括硫酸、盐酸等。Preferably, the acid is an organic acid or an inorganic acid, wherein the organic acid includes p-toluenesulfonic acid, oxalic acid, furandicarboxylic acid, L-malic acid, malonic acid, maleic acid, tartaric acid, etc., and the inorganic acid includes Sulfuric acid, hydrochloric acid, etc.
优选的，所述酸的浓度为0.05M～1M。Preferably, the concentration of the acid is 0.05M-1M.
优选的，所述有机溶剂包括异丁醇、2-甲基四氢呋喃、甲苯、甲基异丁基酮、环戊基甲醚、2-丁醇等。Preferably, the organic solvent includes isobutanol, 2-methyltetrahydrofuran, toluene, methyl isobutyl ketone, cyclopentyl methyl ether, 2-butanol and the like.
优选的，所述有机溶剂和水溶液的加入量之比(体积比)为0.2～5.0。Preferably, the ratio (volume ratio) of the added amount of the organic solvent to the aqueous solution is 0.2-5.0.
优选的，所述木质纤维生物质原料的加入量与有机溶剂和水溶液总体积的液固比为10～30。Preferably, the liquid-solid ratio of the added amount of the lignocellulosic biomass raw material to the total volume of the organic solvent and the aqueous solution is 10-30.
优选的，所述反应温度为80～180℃，反应时间为0.25～8h。Preferably, the reaction temperature is 80-180°C, and the reaction time is 0.25-8h.
优选的，所述反应器可以为置于油浴中的压力反应釜、带磁力搅拌的反应釜、微波反应器中的一种。Preferably, the reactor may be one of a pressure reactor placed in an oil bath, a reactor with magnetic stirring, and a microwave reactor.
本发明的制备方法具有如下优点及有益效果：The preparation method of the present invention has the following advantages and beneficial effects:
(1)本发明可以在基于有机溶剂和水溶液形成的两相体系的基础下一锅法将木质纤维生物质三大组分高选择性拆解。木质素溶解并被抽提到有机溶剂中，半纤维素水解为木糖和阿拉伯糖于水溶液中，纤维素保留在固相残渣中，实现三大组分的同时拆解及组分的定向迁移。(1) The present invention can disassemble the three major components of lignocellulosic biomass with high selectivity in one pot on the basis of a two-phase system formed based on an organic solvent and an aqueous solution. The lignin is dissolved and extracted into the organic solvent, the hemicellulose is hydrolyzed into xylose and arabinose in the aqueous solution, and the cellulose remains in the solid phase residue, realizing the simultaneous disassembly of the three components and the directional migration of the components .
(2)本发明可以分别回收获得生物质三大组分。木质素于有机溶剂中可通过反溶剂法或蒸馏法回收；纤维素残渣通过过滤回收；木糖和阿拉伯糖可从水溶液中浓缩结晶获得。(2) The present invention can separately recover and obtain three major components of biomass. Lignin can be recovered by anti-solvent method or distillation in organic solvent; cellulose residue can be recovered by filtration; xylose and arabinose can be concentrated and crystallized from aqueous solution.
(3)本发明是一种可以放大的反应体系，可同比例扩大反应条件进行反应，反应效果不受影响。(3) The present invention is a reaction system that can be scaled up, and the reaction conditions can be expanded in the same proportion to react, and the reaction effect is not affected.
(4)本发明可通过改变反应的各种条件以达到不同的分离目的，可通过更换不同的有机溶剂进行反应，如异丁醇可以更多地脱除木质素；2-甲基四氢呋喃可更好地保护纤维素；甲苯、甲基异丁基酮和环戊基甲醚可选择性地获得高的半纤维素糖得率，但对木质素脱除较少。(4) The present invention can achieve different separation purposes by changing the various conditions of the reaction, and can react by changing different organic solvents, such as isobutanol, which can remove lignin more; 2-methyltetrahydrofuran can be changed Good protection of cellulose; toluene, methyl isobutyl ketone and cyclopentyl methyl ether can selectively obtain high hemicellulose sugar yield, but less lignin removal.
(5)本发明是一种绿色高效的木质纤维生物质预处理方法，具有反应过程简单、反应效率高的特点。木糖/阿拉伯糖得率为3.12％-100.00％，半纤维素糖得率为6.54％-81.90％，糠醛得率为0.00％-50.75％，半纤维素脱除率为34.25％-98.15％，纤维素保留率为72.26％-97.05％，木质素脱除率为22.59％-89.37％。(5) The present invention is a green and efficient lignocellulosic biomass pretreatment method, which has the characteristics of simple reaction process and high reaction efficiency. The yield of xylose/arabinose is 3.12%-100.00%, the yield of hemicellulose sugar is 6.54%-81.90%, the yield of furfural is 0.00%-50.75%, and the removal rate of hemicellulose is 34.25%-98.15%, The cellulose retention rate is 72.26%-97.05%, and the lignin removal rate is 22.59%-89.37%.
附图说明Description of drawings
图1为本发明所述一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法的工艺流程图。Fig. 1 is a process flow diagram of a method for splitting three major components of biomass based on a one-pot acid hydrolysis pretreatment of a two-phase system according to the present invention.
图2为实施例1反应后水溶液的高效液相色谱图。Fig. 2 is the high performance liquid phase chromatogram of aqueous solution after
图3为实施例2麦草秸秆原料的扫描电镜图。Fig. 3 is a scanning electron micrograph of the wheat straw raw material in Example 2.
图4为实施例2反应后回收残渣的扫描电镜图。Figure 4 is a scanning electron micrograph of the recovered residue after the reaction in Example 2.
具体实施方式Detailed ways
下面结合实施例及附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。The present invention will be further described in detail below in conjunction with the embodiments and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
以下实施例所得的木糖/阿拉伯糖以及糠醛产物的定性及定量通过HPLC测试确定。The quality and quantity of the xylose/arabinose and furfural products obtained in the following examples were determined by HPLC testing.
以下实施例木糖/阿拉伯糖浓度y＝0.0029x*z(mg/L)，式中x为HPLC所测峰面积，y为木糖/阿拉伯糖浓度，z为溶液的稀释倍数，单位mg/L。In the following examples, the xylose/arabinose concentration y=0.0029x*z (mg/L), where x is the peak area measured by HPLC, y is the xylose/arabinose concentration, and z is the dilution factor of the solution, in mg/L L.
以下实施例糠醛浓度b＝0.0024a*z(mg/L)，式中a为HPLC所测峰面积，b为糠醛浓度，z为溶液的稀释倍数，单位mg/L。In the following examples, furfural concentration b=0.0024a*z (mg/L), where a is the peak area measured by HPLC, b is the concentration of furfural, and z is the dilution factor of the solution in mg/L.
实施例1Example 1
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在反应罐中加入1.5g经磨粉抽提后的麦草秸秆原料，15mL水溶液，15mL 2-甲基四氢呋喃溶液，1M对甲苯磺酸。封装于反应釜中，放入已设置并升温到120℃的油浴锅中，反应3h后，将反应釜取出放在冰水浴中快速冷却至室温。得到富含木糖/阿拉伯糖的水溶液，含木质素和少量糠醛的有机溶液，以及剩余含纤维素的固体残渣。Add 1.5g of wheat straw raw material after grinding and extraction, 15mL of aqueous solution, 15mL of 2-methyltetrahydrofuran solution, and 1M p-toluenesulfonic acid into the reaction tank. Package it in a reaction kettle, put it into an oil bath that has been set and heated up to 120°C, and react for 3 hours, take out the reaction kettle and place it in an ice-water bath to quickly cool down to room temperature. An aqueous solution rich in xylose/arabinose, an organic solution containing lignin and a small amount of furfural, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的木糖和阿拉伯糖质量之和)×100％Hemicellulose sugar yield=(sum of xylose and arabinose quality in solution after reaction/sum of xylose and arabinose quality in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例水相经稀释后于液相测试，测试的出峰图见图2。11.627为葡萄糖；12.496为木糖；13.477为阿拉伯糖；49.805为糠醛，将峰面积带入上述公式进行计算，可得76.15％的木糖得率，100％的阿拉伯糖得率，半纤维素糖得率为81.90％，以及3.35％的糠醛得率。并且该实施例有75.88％的木质素脱除率，89.37％的半纤维素脱除率，以及92.37％的纤维素保留率。In this example, the water phase was diluted and then tested in the liquid phase. The peak output of the test is shown in Figure 2. 11.627 is glucose; 12.496 is xylose; 13.477 is arabinose; The yield of xylose was 76.15%, the yield of arabinose was 100%, the yield of hemicellulose sugar was 81.90%, and the yield of furfural was 3.35%. And this embodiment has a lignin removal rate of 75.88%, a hemicellulose removal rate of 89.37%, and a cellulose retention rate of 92.37%.
实施例2Example 2
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在反应罐中加入1.5g经磨粉抽提后的麦草秸秆原料，15mL水溶液，15mL 2-甲基四氢呋喃溶液，0.2M对甲苯磺酸。封装于反应釜中，放入已设置并升温到180℃的油浴锅中，反应3h后，将反应釜取出放在冰水浴中快速冷却至室温。得到富含木糖/阿拉伯糖水溶液，含木质素和糠醛的有机溶液，以及剩余含纤维素的固体残渣。Add 1.5g of wheat straw raw material after grinding and extraction, 15mL of aqueous solution, 15mL of 2-methyltetrahydrofuran solution, and 0.2M p-toluenesulfonic acid into the reaction tank. Package it in a reaction kettle, put it into an oil bath that has been set and heated to 180°C, and react for 3 hours, take out the reaction kettle and place it in an ice-water bath to quickly cool to room temperature. An aqueous solution rich in xylose/arabinose, an organic solution containing lignin and furfural, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的糖质量)×100％Hemicellulose sugar yield=(sum of xylose and arabinose mass in solution after reaction/sugar mass in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例可获得32.48％木糖得率，71.12％的阿拉伯糖得率，半纤维素糖得率为35.06％，以及50.75％的糠醛得率；并且有78.26％的木质素脱除率，98.15％的半纤维素脱除率，以及72.26％的纤维素保留率。图3和图4可以对比看出：图4的形貌被严重破坏，看不出原有的纤维形态，此时反应条件剧烈，无定型区的木质素和半纤维素可充分被脱除，并且也导致了纤维素的较多脱除，保留率降低。This embodiment can obtain 32.48% xylose yield, 71.12% arabinose yield, hemicellulose sugar yield is 35.06%, and 50.75% furfural yield; And there is 78.26% lignin removal rate, 98.15 % hemicellulose removal rate, and 72.26% cellulose retention rate. From Figure 3 and Figure 4, it can be seen that the morphology of Figure 4 is severely damaged, and the original fiber shape cannot be seen. At this time, the reaction conditions are severe, and the lignin and hemicellulose in the amorphous area can be fully removed. And also lead to more removal of cellulose, lower retention rate.
实施例3Example 3
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在聚四氟乙烯反应罐中加入1.5g经磨粉抽提后的木材原料，15mL水溶液，15mL 2-甲基四氢呋喃溶液，0.1M硫酸。封装于反应釜中，放入已设置并升温到100℃的微波反应器中，反应0.5h后，将反应釜取出放在冰水浴中快速冷却至室温。得到含木糖/阿拉伯糖水溶液，含木质素的有机溶液，以及剩余含纤维素的固体残渣。Add 1.5g of milled and extracted wood raw material, 15mL of aqueous solution, 15mL of 2-methyltetrahydrofuran solution, and 0.1M sulfuric acid into a polytetrafluoroethylene reaction tank. Package it in a reaction kettle, put it into a microwave reactor that has been set and heated up to 100°C, and react for 0.5h, take out the reaction kettle and place it in an ice-water bath to quickly cool down to room temperature. An aqueous solution containing xylose/arabinose, an organic solution containing lignin, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的糖质量)×100％Hemicellulose sugar yield=(sum of xylose and arabinose mass in solution after reaction/sugar mass in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例可获得38.53％的木糖得率，82.53％的阿拉伯糖得率，半纤维素糖得率为42.47％，糠醛得率为0.00％。并且有41.78％的木质素脱除率，67.67％的半纤维素脱除率，以及91.81％的纤维素保留率。In this embodiment, the yield of xylose is 38.53%, the yield of arabinose is 82.53%, the yield of hemicellulose sugar is 42.47%, and the yield of furfural is 0.00%. And there are 41.78% lignin removal rate, 67.67% hemicellulose removal rate, and 91.81% cellulose retention rate.
实施例4Example 4
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在聚四氟乙烯反应罐中加入1.5g经磨粉抽提后的木材原料，10mL水溶液，20mL异丁醇溶液，0.1M对甲苯磺酸。封装于反应釜中，放入已设置并升温到100℃的微波反应器中，反应1h后，将反应釜取出放在冰水浴中快速冷却至室温。得到含木糖/阿拉伯糖水溶液，含木质素的有机溶液，以及剩余含纤维素的固体残渣。Add 1.5g of milled and extracted wood raw material, 10mL of aqueous solution, 20mL of isobutanol solution, and 0.1M p-toluenesulfonic acid into a polytetrafluoroethylene reaction tank. Package it in a reaction kettle, put it into a microwave reactor that has been set and heated up to 100°C, and after reacting for 1 hour, take out the reaction kettle and place it in an ice-water bath to quickly cool it to room temperature. An aqueous solution containing xylose/arabinose, an organic solution containing lignin, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的糖质量)×100％Hemicellulose sugar yield=(sum of xylose and arabinose mass in solution after reaction/sugar mass in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例可获得48.06％的木糖得率，95.41％的阿拉伯糖得率，半纤维素糖得率为51.30％，糠醛得率为0.16％。并且有75.78％的木质素脱除率，65.67％的半纤维素脱除率，以及87.81％的纤维素保留率。In this embodiment, the yield of xylose is 48.06%, the yield of arabinose is 95.41%, the yield of hemicellulose sugar is 51.30%, and the yield of furfural is 0.16%. And there are 75.78% lignin removal rate, 65.67% hemicellulose removal rate, and 87.81% cellulose retention rate.
实施例5Example 5
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在聚四氟乙烯反应罐中加入0.5g经磨粉抽提后的玉米原料，5mL水溶液，5mL异丁醇溶液，0.2M草酸。封装于反应釜中，放入已设置并升温到140℃的油浴锅中，反应4h后，将反应釜取出放在冰水浴中快速冷却至室温。得到含木糖/阿拉伯糖水溶液，含木质素的有机溶液，以及剩余含纤维素的固体残渣。Add 0.5 g of milled and extracted corn raw material, 5 mL of aqueous solution, 5 mL of isobutanol solution, and 0.2 M oxalic acid into a polytetrafluoroethylene reaction tank. Package it in a reaction kettle, put it into an oil bath that has been set and heated up to 140°C, and react for 4 hours, take out the reaction kettle and place it in an ice-water bath to quickly cool down to room temperature. An aqueous solution containing xylose/arabinose, an organic solution containing lignin, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的糖质量)×100％Hemicellulose sugar yield=(sum of xylose and arabinose mass in solution after reaction/sugar mass in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例可获得16.70％的木糖得率，78.22％的阿拉伯糖得率，半纤维素糖得率为39.27％，糠醛得率为0.00％。并且有47.76％的木质素脱除率，67.24％的半纤维素脱除率，以及91.34％的纤维素保留率。In this embodiment, the yield of xylose is 16.70%, the yield of arabinose is 78.22%, the yield of hemicellulose sugar is 39.27%, and the yield of furfural is 0.00%. And there are 47.76% lignin removal rate, 67.24% hemicellulose removal rate, and 91.34% cellulose retention rate.
实施例6Example 6
本实施例的一种基于两相体系的一锅法酸水解预处理拆分生物质三大组分的方法，具体制备步骤如下：In this embodiment, a method for splitting the three major components of biomass based on the one-pot acid hydrolysis pretreatment of the two-phase system, the specific preparation steps are as follows:
在聚四氟乙烯反应罐中加入1.5g经磨粉抽提后的麦草秸秆原料，15mL水溶液，15mL环戊基甲醚溶液，0.1M对甲苯磺酸。封装于反应釜中，放入已设置并升温到140℃的磁力搅拌反应釜中反应3h后，将反应釜取出放在冰水浴中快速冷却至室温。得到含木糖/阿拉伯糖水溶液，含木质素的有机溶液，以及剩余含纤维素的固体残渣。Add 1.5 g of wheat straw raw material after milling and extraction, 15 mL of aqueous solution, 15 mL of cyclopentyl methyl ether solution, and 0.1 M p-toluenesulfonic acid into a polytetrafluoroethylene reaction tank. Packaged in a reaction kettle, put it into a magnetically stirred reaction kettle that has been set and heated to 140°C for 3 hours of reaction, then take out the reaction kettle and place it in an ice-water bath to quickly cool down to room temperature. An aqueous solution containing xylose/arabinose, an organic solution containing lignin, and a solid residue containing cellulose are obtained.
溶液中木糖/阿拉伯糖含量由高效液相色谱仪(HPLC)测定。The content of xylose/arabinose in the solution was determined by high performance liquid chromatography (HPLC).
半纤维素糖得率＝(反应后溶液中的木糖和阿拉伯糖质量之和/反应前原料中的糖质量)×100％Hemicellulose sugar yield=(sum of xylose and arabinose mass in solution after reaction/sugar mass in raw material before reaction)×100%
糠醛得率＝(反应后溶液中的糠醛摩尔质量/反应前原料中的木糖和阿拉伯糖摩尔质量之和)×100％Furfural yield=(molar mass of furfural in solution after reaction/sum of molar mass of xylose and arabinose in raw material before reaction)×100%
木质素脱除率＝(反应前原料中的木质素质量–反应后剩余木质素质量)/反应前原料中的木质素质量×100％Lignin removal rate = (quality of lignin in raw material before reaction – quality of remaining lignin after reaction) / quality of lignin in raw material before reaction × 100%
半纤维素脱除率＝(反应前原料中的半纤维素质量–反应后剩余半纤维素质量)/反应前原料中的半纤维素质量×100％Hemicellulose removal rate = (mass of hemicellulose in raw material before reaction - mass of remaining hemicellulose after reaction)/mass of hemicellulose in raw material before reaction × 100%
纤维素保留率＝反应后纤维素质量/反应前原料中的纤维素质量×100％Cellulose retention rate = mass of cellulose after reaction / mass of cellulose in raw material before reaction × 100%
本实施例可获得61.41％的木糖得率，100％的阿拉伯糖得率，半纤维素糖得率为65.32％，糠醛得率为0.00％。并且有29.32％的木质素脱除率，80.68％的半纤维素脱除率，以及97.05％的纤维素保留率。In this embodiment, the yield of xylose is 61.41%, the yield of arabinose is 100%, the yield of hemicellulose sugar is 65.32%, and the yield of furfural is 0.00%. And there are 29.32% lignin removal rate, 80.68% hemicellulose removal rate, and 97.05% cellulose retention rate.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above-mentioned embodiment, and any other changes, modifications, substitutions, combinations, Simplifications should be equivalent replacement methods, and all are included in the protection scope of the present invention.
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| CN107385119A (en) * | 2017-08-28 | 2017-11-24 | 华南理工大学 | A kind of method that corncob rapidly and efficiently prepares xylose hydrolysis fluid |
| CN111395025A (en) * | 2020-04-07 | 2020-07-10 | 齐鲁工业大学 | A kind of comprehensive utilization method of lignocellulosic biomass |
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| CN107385119A (en) * | 2017-08-28 | 2017-11-24 | 华南理工大学 | A kind of method that corncob rapidly and efficiently prepares xylose hydrolysis fluid |
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