技术领域technical field
本发明涉及一种多羟基质子型铵盐类离子液体溶解分离木质纤维素秸秆原料中的纤维素和木质素、半纤维素，获得高纯度纤维素Ⅰ型材料，属于生物质领域。The invention relates to a polyhydroxy proton type ammonium salt ionic liquid which dissolves and separates cellulose, lignin and hemicellulose in lignocellulose straw raw materials to obtain high-purity cellulose type I materials, belonging to the field of biomass.
背景技术Background technique
随着地球化石资源的日益衰竭，能源与环境问题已经成为人类工业化发展中亟需解决的重要难题，开发并使用绿色可再生资源，实现资源的高效利用是解决当前化学工业发展缓慢的有效途径。生物质资源作为地球上储量大、分布广的绿色可再生能源，在近些年的研究探索中受到了人们的广泛关注。除了森林植被以外，农作物秸秆和多种一年生的植物秸秆也在自然界的物质与能量循环中发挥着重要作用。作为生物质资源的主要组成部分，纤维素，半纤维素和木质素可以通过生物质精炼的工艺进行提取并加以利用。纤维素(35-55％)和半纤维素(20-35％)可以分解为葡萄糖和木糖，并通过生物和化学的方法转化制取多种药物中间体和燃料乙醇、汽油、以及二醇等化学品，而木质素(15-30％)也可以通过不同方法催化转化为汽油和其它高附加值的芳香族化合物。玉米秸秆、棉秆、芦苇杆和木屑这些低成本的农业废弃物，其本身的木质纤维素是自然界中宝贵的可再生资源。With the depletion of fossil resources on the earth, energy and environmental issues have become important problems that need to be solved in the development of human industrialization. The development and use of green renewable resources and the efficient use of resources are effective ways to solve the current slow development of the chemical industry. Biomass resources, as a green renewable energy with large reserves and wide distribution on the earth, have received extensive attention in research and exploration in recent years. In addition to forest vegetation, crop stalks and various annual plant stalks also play an important role in the material and energy cycle in nature. As the main components of biomass resources, cellulose, hemicellulose and lignin can be extracted and utilized through biomass refining processes. Cellulose (35-55%) and hemicellulose (20-35%) can be decomposed into glucose and xylose, and converted into various pharmaceutical intermediates and fuel ethanol, gasoline, and glycols through biological and chemical methods and other chemicals, while lignin (15-30%) can also be catalytically converted into gasoline and other high value-added aromatic compounds by different methods. Corn stalks, cotton stalks, reed stalks and sawdust are low-cost agricultural wastes, and their lignocellulose is a valuable renewable resource in nature.
通过对木质纤维素复杂结构进行溶解分离预处理，实现生物质组分纤维素和半纤维素、木质素的高效分离是生物质资源利用的关键步骤，其中，对于纤维素的分离提取及利用尤为重要。传统预处理工艺过程所用的溶剂多为酸、碱溶液或者有机溶剂，但是这些溶剂体系普遍存在环境污染严重、不能回收利用、对设备要求严格和成本高等问题。It is a key step in the utilization of biomass resources to realize the efficient separation of biomass components cellulose, hemicellulose and lignin by dissolving and separating the complex structure of lignocellulose. Among them, the separation, extraction and utilization of cellulose are particularly important. important. The solvents used in the traditional pretreatment process are mostly acids, alkali solutions or organic solvents, but these solvent systems generally have problems such as serious environmental pollution, non-recyclability, strict requirements on equipment, and high cost.
离子液体作为反应介质和溶剂，在近些年的研究中受到了人们的广泛关注。离子液体具有热稳定性好，难挥发，可回收循环利用等优点，已经广泛应用于有机合成，工业催化和萃取分离等领域。室温离子液体能够与生物质组分形成较强的离子液体氢键作用，这为其应用于生物质的组分溶解分离提供了新思路。常规的单一离子液体溶解分离木质纤维素组分有两种思路，一种思路是用溶解纤维素能力较好的离子液体溶解木质纤维素中的纤维素，然后再生得到无定形态的纤维素Ⅱ型材料，以促进纤维素的进一步转化应用，专利US2010/0163018 A1,WO2016/116126 A2,US2016/0002358 A1均公布了用不同离子液体预处理分离和利用木质纤维素的方法。另一种思路为使用对木质素溶解较好的离子液体去除生物质组分中的木质素，得到富纤维素材料，专利CN 103031762 A则用了这种方法。Ionic liquids, as reaction media and solvents, have received extensive attention in recent years. Ionic liquids have the advantages of good thermal stability, low volatility, and recyclability, and have been widely used in organic synthesis, industrial catalysis, extraction and separation, and other fields. Room temperature ionic liquids can form strong ionic liquid hydrogen bonds with biomass components, which provides a new idea for their application in the dissolution and separation of biomass components. There are two ways of dissolving and separating lignocellulose components in conventional single ionic liquids. One way is to use ionic liquids with better cellulose dissolving ability to dissolve cellulose in lignocellulose, and then regenerate to obtain amorphous cellulose II Type materials to promote the further conversion and application of cellulose. Patents US2010/0163018 A1, WO2016/116126 A2, and US2016/0002358 A1 all disclose methods for separating and utilizing lignocellulose by pretreatment with different ionic liquids. Another idea is to use ionic liquids that can dissolve lignin better to remove lignin from biomass components to obtain cellulose-rich materials. Patent CN 103031762 A uses this method.
离子液体用于生物质组分溶解的阳离子主要包括N-甲基咪唑类、铵盐类和磷盐类，阴离子主要为X-(卤素)、CH3COO-、CH3SO4-、(CH3)2O2PO2-和HCO2-等，然而大多数单一离子液体不能实现木质纤维素组分中纤维素和半纤维素的高效分离，并且合成步骤较多，成本高，通过溶解并再生得到的纤维素材料会破坏原材料中纤维素的晶型结构，在后续的应用中受到限制，同时，溶解分离中使用二甲基亚砜有机溶剂，环境污染严重，不符合可持续发展和绿色过程工程的理念。The cations used for the dissolution of biomass components in ionic liquids mainly include N-methylimidazoles, ammonium salts and phosphorus salts, and the anions are mainly X- (halogen), CH3 COO- , CH3 SO4- , (CH3 )2 O2 PO2- and HCO2- , etc. However, most single ionic liquids cannot achieve efficient separation of cellulose and hemicellulose in lignocellulosic components, and there are many synthesis steps and high cost. The regenerated cellulose material will destroy the crystalline structure of cellulose in the raw material, which is limited in subsequent applications. At the same time, the use of dimethyl sulfoxide organic solvent in the dissolution and separation causes serious environmental pollution and does not meet sustainable development and green Concept of process engineering.
发明内容Contents of the invention
本发明提供了一种多羟基质子型铵盐类离子液体作为溶解分离木质纤维素组分的溶剂，一步法能使生物质原料中的木质素和半纤维素同时去除，得到较高纯度的Ⅰ型纤维素材料。离子液体结构通式如下：The invention provides a polyhydroxy proton type ammonium salt ionic liquid as a solvent for dissolving and separating lignocellulose components, which can simultaneously remove lignin and hemicellulose in biomass raw materials to obtain relatively high-purity I type cellulose material. The general structure of ionic liquid is as follows:
本发明所用的离子液体合成方法如下：The synthetic method of ionic liquid used in the present invention is as follows:
在273.15K温度条件下，将适量甲烷磺酸通过恒压滴定漏斗缓慢滴入醇胺的甲醇溶液中，滴加完毕后，升温至室温反应48h，停止反应，旋转蒸发除去甲醇溶剂，分别用乙醚和乙酸乙酯洗涤三次，最后将合成的离子液体真空干燥。Under the temperature condition of 273.15K, slowly drop an appropriate amount of methanesulfonic acid into the methanol solution of alcoholamine through a constant pressure titration funnel. and ethyl acetate three times, and finally the synthesized ionic liquid was vacuum-dried.
对木质纤维素的溶解分离实验步骤如下：The experimental steps for dissolving and separating lignocellulose are as follows:
将原料生物质秸秆先用中性洗涤剂洗涤，干燥，粉碎和过筛，筛选出一定粒径大小(≤0.125mm)的木质纤维素原料。The raw material biomass straw is firstly washed with a neutral detergent, dried, pulverized and sieved, and the lignocellulose raw material with a certain particle size (≤0.125 mm) is screened out.
将质量分数5％-10％的木质纤维素原料和离子液体同时加入烧瓶中加热搅拌。The lignocellulosic raw material and the ionic liquid with a mass fraction of 5%-10% are simultaneously added into the flask, heated and stirred.
实验温度为80-160℃,反应时间为0.25-24h，每隔0.5h在偏光显微镜下观察木质纤维素组分溶解状况。反应结束后，向体系中加入10mL去离子水稀释离心，将离心得到的固体水洗3-6次，干燥得到高纯度纤维素材料。The experimental temperature is 80-160°C, the reaction time is 0.25-24h, and the dissolving state of the lignocellulose component is observed under a polarizing microscope every 0.5h. After the reaction, add 10 mL of deionized water to the system to dilute and centrifuge, wash the centrifuged solid with water for 3-6 times, and dry to obtain a high-purity cellulose material.
本发明优势Advantages of the invention
1发明的离子液体合成简单，原料价格低廉，克服了常规离子液体价格昂贵，合成方法繁琐，成本高等缺点。1. The ionic liquid of the invention is simple to synthesize, and the price of raw materials is low, which overcomes the disadvantages of conventional ionic liquids such as high price, cumbersome synthesis method and high cost.
2发明的离子液体对木质纤维素表现出了优异的溶解分离能力，能同时溶解木质纤维素组分中的木质素和半纤维素，得到纯度为70-95％的纤维素Ⅰ型材料，保持了秸秆原料中纤维素的晶型结构。2. The ionic liquid of the invention shows excellent dissolving and separating ability for lignocellulose, and can simultaneously dissolve lignin and hemicellulose in the lignocellulose component to obtain cellulose type I material with a purity of 70-95%. The crystal structure of cellulose in straw raw materials was determined.
3双羟基类离子液体溶解分离效果最好，同时，实验中纤维素不溶解，产物易于分离，能耗低，为离子液体分离生物质组分工业化提供了可能。3 Dihydroxy ionic liquids have the best dissolution and separation effect. At the same time, in the experiment, the cellulose was not dissolved, the product was easy to separate, and the energy consumption was low, which provided the possibility for the industrialization of the separation of biomass components by ionic liquids.
4发明中溶解分离实验只用了离子液体和水，省去了常规离子液体溶解分离秸秆不同组分所使用的二甲基亚砜稀释剂，更加绿色环保，符合绿色过程工程的理念。4. In the dissolution and separation experiment of the invention, only ionic liquid and water are used, which saves the dimethyl sulfoxide diluent used in the conventional ionic liquid to dissolve and separate different components of straw, which is more green and environmentally friendly, and conforms to the concept of green process engineering.
附图说明Description of drawings
附图为具体实施例1，实施例2，实施例3，实施例4，实施例5，实施例6，实施例7的纤维素材料和秸秆原料与棉杆原料的XRD对比图。Accompanying drawing is specific embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, the XRD contrast chart of the cellulose material of embodiment 7 and straw raw material and cotton stalk raw material.
图1具体实施例1，实施例2，实施例3，实施例4，实施例5，实施例6，实施例8，实施例9，实施例10，实施例11的纤维素材料和玉米秸秆原料XRD对比图。Fig. 1 specific embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, embodiment 8, embodiment 9, embodiment 10, the cellulose material of embodiment 11 and corn stalk raw material XRD comparison chart.
图2具体实施例7的纤维素材料和棉秆原料XRD对比图。Fig. 2 is a comparison chart of XRD of the cellulose material and cotton stalk raw material of specific example 7.
具体实施方式detailed description
下面结合实施例进一步说明本发明，但是，具体实施例子在任何方面都不构成对本发明范围的限制。The present invention will be further described below in conjunction with the examples, but the specific implementation examples do not constitute a limitation to the scope of the present invention in any respect.
实施例1Example 1
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，120℃条件下磁力搅拌24h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到1.99％，半纤维素含量从31.21％下降到4.04％，纤维素含量从50.53％提高到91.81％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 120° C. for 24 hours, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 1.99%, the hemicellulose content decreased from 31.21% to 4.04%, and the cellulose content increased from 50.53% to 91.81%.
实施例2Example 2
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，120℃条件下磁力搅拌0.25h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到5.30％，半纤维素含量从31.21％下降到10.08％，纤维素含量从50.53％提高到76.53％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 120°C for 0.25h, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 5.30%, the hemicellulose content decreased from 31.21% to 10.08%, and the cellulose content increased from 50.53% to 76.53%.
实施例3Example 3
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，80℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到8.14％，半纤维素含量从31.21％下降到12.60％，纤维素含量从50.53％提高到70.00％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically for 6 hours at 80° C., add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 8.14%, the hemicellulose content decreased from 31.21% to 12.60%, and the cellulose content increased from 50.53% to 70.00%.
实施例4Example 4
向经过干燥的10g质子型离子液体溶剂三乙醇胺甲烷磺酸盐([(HOCH2CH2)3NH]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，160℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到5.45％，半纤维素含量从31.21％下降到5.44％，纤维素含量从50.53％提高到82.44％。Add 0.5g to the dried 10g protic ionic liquid solvent triethanolamine methanesulfonate ([(HOCH2 CH2 )3 NH]+ CH3 SO4- ), wash, dry and sieve (≤0.125mm) The corn stalk powder was stirred magnetically at 160° C. for 6 h, and 10 mL of deionized water was added to the reacted ionic liquid and straw mixture for dilution and centrifuged. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 5.45%, the hemicellulose content decreased from 31.21% to 5.44%, and the cellulose content increased from 50.53% to 82.44%.
实施例5Example 5
向经过干燥的10g质子型离子液体溶剂N,N-二甲基乙醇胺甲烷磺酸盐([(HOCH2CH2)NH(CH3)2]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，140℃条件下磁力搅拌6h，向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到12.51％，半纤维素含量从31.21％下降到9.56％，纤维素含量从50.53％提高到78.01％。Add0.5gofwashed___ , dried and sieved (≤0.125mm) corn stalk powder, magnetically stirred at 140° C. for 6 h, added 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuged. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 12.51%, the hemicellulose content decreased from 31.21% to 9.56%, and the cellulose content increased from 50.53% to 78.01%.
实施例6Example 6
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入1.0g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，130℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到8.60％，半纤维素含量从31.21％下降到8.05％，纤维素含量从50.53％提高到76.10％。Add1.0gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 130° C. for 6 hours, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. The results of component analysis showed that the lignin content in the product decreased from 15.28% to 8.60%, the hemicellulose content decreased from 31.21% to 8.05%, and the cellulose content increased from 50.53% to 76.10%.
实施例7Example 7
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的棉秆粉末，130℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的23.59％下降到16.60％，半纤维素含量从18.45％下降到2.05％，纤维素含量从43.98％提高到75.10％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) cotton stalk powder, stir magnetically at 130° C. for 6 hours, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 23.59% to 16.60%, the hemicellulose content decreased from 18.45% to 2.05%, and the cellulose content increased from 43.98% to 75.10%.
实施例8Example 8
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)3NH]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，150℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到7.22％，半纤维素含量从31.21％下降到9.10％，纤维素含量从50.53％提高到83.32％。To the dried 10g protic ionic liquid solvent N-methyldiethanolamine methanesulfonate ([(HOCH2 CH2 )3 NH]+ CH3 SO4- ), add 0.5 g of washed, dried and sieved ( ≤0.125mm) of corn stalk powder, stirred magnetically for 6 hours at 150°C, added 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuged. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 7.22%, the hemicellulose content decreased from 31.21% to 9.10%, and the cellulose content increased from 50.53% to 83.32%.
实施例9Example 9
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，120℃条件下磁力搅拌0.75h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到4.16％，半纤维素含量从31.21％下降到8.62％，纤维素含量从50.53％提高到82.05％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 120° C. for 0.75 h, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. The results of component analysis showed that the lignin content in the product decreased from 15.28% to 4.16%, the hemicellulose content decreased from 31.21% to 8.62%, and the cellulose content increased from 50.53% to 82.05%.
实施例10Example 10
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.5g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，120℃条件下磁力搅拌1h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到4.03％，半纤维素含量从31.21％下降到8.51％，纤维素含量从50.53％提高到82.25％。Add0.5gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 120° C. for 1 h, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 4.03%, the hemicellulose content decreased from 31.21% to 8.51%, and the cellulose content increased from 50.53% to 82.25%.
实施例11Example 11
向经过干燥的10g质子型离子液体溶剂N-甲基二乙醇胺甲烷磺酸盐([(HOCH2CH2)2NH(CH3)]+CH3SO4-)中加入0.8g经过洗涤、干燥、过筛(≤0.125mm)的玉米秸秆粉末，130℃条件下磁力搅拌6h,向反应后的离子液体和秸秆混合物中加入10mL去离子水稀释、离心分离。将所得未溶解产品使用清水清洗、干燥、称重，计算该离子液体的溶解度，并将产品进行木质纤维素组分分析。组分分析结果显示，产品中木质素含量从原料的15.28％下降到7.31％，半纤维素含量从31.21％下降到7.66％，纤维素含量从50.53％提高到75.10％。Add0.8gofwashedanddried_ 1. Sieve (≤0.125mm) corn stalk powder, stir magnetically at 130° C. for 6 hours, add 10 mL of deionized water to the reacted ionic liquid and straw mixture for dilution, and centrifuge. The obtained undissolved product is washed with clear water, dried and weighed, the solubility of the ionic liquid is calculated, and the product is subjected to lignocellulose component analysis. Component analysis results showed that the lignin content in the product decreased from 15.28% to 7.31%, the hemicellulose content decreased from 31.21% to 7.66%, and the cellulose content increased from 50.53% to 75.10%.
| Application Number | Priority Date | Filing Date | Title |
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| CN201611261727.0ACN106702800B (en) | 2016-12-30 | 2016-12-30 | A method for removing straw lignin and hemicellulose with proton-type ionic liquid |
| Application Number | Priority Date | Filing Date | Title |
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| CN201611261727.0ACN106702800B (en) | 2016-12-30 | 2016-12-30 | A method for removing straw lignin and hemicellulose with proton-type ionic liquid |
| Publication Number | Publication Date |
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| CN106702800Atrue CN106702800A (en) | 2017-05-24 |
| CN106702800B CN106702800B (en) | 2019-02-26 |
| Application Number | Title | Priority Date | Filing Date |
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| CN201611261727.0AActiveCN106702800B (en) | 2016-12-30 | 2016-12-30 | A method for removing straw lignin and hemicellulose with proton-type ionic liquid |
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| WO1994023009A1 (en)* | 1993-03-31 | 1994-10-13 | Unilever N.V. | Liquid cleaning products |
| CN101671259A (en)* | 2009-09-28 | 2010-03-17 | 中国科学院过程工程研究所 | Synthesis of alcoholamines functionalized ionic liquid |
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| CN105229224A (en)* | 2013-03-15 | 2016-01-06 | 帝国革新有限公司 | Process |
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| CN111154817A (en)* | 2020-02-19 | 2020-05-15 | 中国科学院过程工程研究所 | A method for efficient separation and enzymatic hydrolysis of lignocellulose in an ionic liquid-high-boiling alcohol composite system |
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| CN113774701A (en)* | 2021-09-16 | 2021-12-10 | 江南大学 | Method for removing lignin in straw by using glycine and acetic acid |
| CN113882179A (en)* | 2021-09-29 | 2022-01-04 | 江南大学 | A method for removing lignin from straw by utilizing 1-hydroxy-3-mercaptopropane-2-amine nitrate |
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