微波辅助[Bmim]FeCl_3Br催化稻草秸秆纤维素水解为还原糖的研究

本文研究了稻草秸秆在微波辅助、离子液体Bmim]FeCl3Br中水解为还原糖的条件。在微波功率为240W,物料/催化剂比为5∶4g·g-1,微波处理时间为130min,物料/水比为1∶40g·mL-1的条件下,还原糖收率为28.06%。     

超声波-微波辅助柠檬酸催化纤维素水解条件

以柠檬酸为催化剂,采用超声波-微波相结合的辅助手法对自制稻草纤维素进行了水解研究。以还原糖得率为指标,在单因素试验的基础上,通过3因素3水平的正交试验考察了酸浓度、超声波处理时间和微波加热时间对指标的影响。对实验结果进行了极差分析和方差分析,结果表明,最佳反应条件为：柠檬酸浓度20%、超声波处理90 min、微波500 W加热30 min,此时还原糖得率最高,达64.46%。对稻草纤维素原料和水解残渣进行了红外表征,结果显示,水解残渣仍以纤维素的形式存在,可重新水解,提高原料利用率。     

纤维素酶水解纤维素还原糖的测定

对不同类菌种在不同培养基中的酶活性进行比较,测定了其底物得糖率,最高达８．５９％,可对纤维素酶的进一步研究提供实验参照。     

［Bmim］Cl离子液体中微波辐射加热促进稻草秸秆酸水解制备还原糖

以［Bmim］Cl离子液体为介质,研究了微波辐射加热对硫酸催化稻草秸秆水解的促进作用,并对水解产物中的还原糖进行了测定。着重考察了［Bmim］Cl离子液体用量、硫酸浓度、反应温度和反应时间等因素对还原糖收率的影响,并采用正交试验法对微波辐射下稻草酸水解条件进行了优化。结果表明,在［Bmim］Cl离子液体介质中,用微波辐射加热促进稻草酸水解制备还原糖的最佳条件是：［Bmim］Cl用量10.0ml,硫酸浓度10.0%,微波加热温度85℃,反应时间60 min。在此条件下还原糖的收率可达到23. 22%,而常规酸水解得到的还原糖收率仅为18.74%。通过显微镜和红外光谱对水解残余物与稻草原料进行分析后发现：水解后的稻草残渣变细、变薄,并且与稻草原料的结构基本一致,保留了较好的纤维素特征。     

稻草纤维素水解机理及工艺条件的研究

以稻草秸杆为纤维素原料,用2%氢氧化钠对其进行预处理,选用纤维素酶作为催化剂对纤维素进行酶法水解,采用DNS法测定纤维素水解液还原糖的含量,并计算其糖化率。探讨了纤维素酶水解稻草秸秆纤维素的反应机理,研究了纤维素酶的添加量、反应温度、pH、反应时间、振荡等因素对稻草纤维素酶水解的影响。实验结果表明,当固液比为1∶30、纤维素酶添加量为40 mg、50℃、pH 4.8、振荡反应12h,纤维素酶解液的糖化率可达40%。     

微波辐射下盐酸催化纤维素水解研究

采用微波辐射与盐酸催化相结合对纤维素进行水解,探讨了微波功率、酸浓度和反应时间等工艺条件对纤维素水解过程的影响,在微波功率为500 W,盐酸浓度为20%的条件下,反应50 min水解液中还原糖浓度达到最大值36.7 g·L-1,比平行实验中常规水浴加热所得还原糖浓度提高了14.4 g·L-1.对微波条件和常规条件下水解残余物的红外分析表明,微波条件与常规条件下的水解残余物结构基本一致,保留了很好的纤维素特征.     

多孔秸秆碳磺酸催化纤维素水解研究

以玉米秸秆为原料、NaOH为造孔剂,采用碳化-活化制备多孔秸秆碳磺酸(PSCSA),用于纤维素的水解。通过X射线衍射(XRD)、傅里叶红外光谱(FTIR)、N₂吸脱附分析(BET)、扫描电子显微镜(SEM)等对PSCSA进行表征分析,表明PSCSA为不定形碳结构并有部分微弱的石墨结晶,含有羟基(-OH)、羧基(-COOH)、磺酸基(-SO₃H),且表面为多孔形貌。在多孔秸秆碳磺酸添加量为2.5g·g^-1(纤维素)、底物纤维素浓度为3mg·m L^-1、190℃水解1h的条件下,多孔秸秆碳磺酸催化纤维素水解还原糖得率可达60.61%。     

微波辐射对硫酸催化稻草水解的促进作用

研究了微波辐射对硫酸催化稻草水解的促进作用.考察了微波辐射功率、辐射时间、硫酸质量分数及每升硫酸溶液中稻草添加量对还原糖得率的影响.与常规酸水解比较,微波辐射可显著加快水解速率,缩短糖化时间.采用正交试验法对微波辐射下稻草硫酸水解条件进行了优化,最佳条件为:微波功率280 W,辐射时间30 min,硫酸质量分数25%,每升硫酸溶液中稻草添加量30 g,还原糖得率达到26.5%.     

微波水解法制备稻草微晶纤维素及能效分析

优化了微波水解法降解稻草纤维制备微晶纤维素(MCC)的反应条件。结果表明,当盐酸质量分数为6%、反应时间为10 min、微波功率为231 W、固液比为1∶20(g∶mL)时,MCC的产率达87.00%,而能耗仅为常规加热法的23.1%。微观分析证实,微波水解降低了纤维素分子的聚合度,增强了对稻草纤维束非晶区结构的破坏作用,提高了产物的结晶度,但纤维素分子特征并未发生改变。     

纤维素酶水解纤维素还原糖的测定

对不同类菌种在不同培养基中的酶活性进行比较,测定了其底物得糖率,最高达８．５９％。可对纤维素酶的进一步研究提供实验参照。     

纤维素的酶水解糖化

纤维素为自然界存在最多的再生有机资源，能水解成葡萄糖，加工成食品、燃料、化工产品等。酸和酶都能催化水解，但酶法效果好，所得水解液的纯度高。多年来对于纤维素的酶法水解研究工作很多，但还有若干问题有待解决，尚未发展成适于工业生产应用的好工艺。本文扼要地综述纤维素的酶水解机理和纤维素物料的应用工艺。纤维素酶系内切葡聚糖酶、外切葡聚糖酶和β-葡萄糖甙酶的混合物，这三种酶协同起水解作用。纤维素物料不纯，还有伴生物半纤维素和木质素共同存在，需要预先处理，破坏纤维素的结晶性，提高水解效能，分离开半纤维素和木质素，加以好的利用，提高经济效益。     

微波辅助棉花秸秆稀酸水解糖化工艺研究

采用微波辅助稀酸法对棉花秸秆进行水解糖化。探索了微波辐射温度、微波辐射时间、料液比及硫酸浓度对秸秆水解糖化效果的影响。结果表明,微波辅助棉花秸秆稀酸水解糖化的最佳糖化工艺条件为:微波辐射温度80℃,微波辐射时间50min,料液比1∶16g/mL,硫酸浓度3.0%。各影响因素对还原糖收率的影响顺序为:料液比微波辐射温度硫酸浓度微波辐射时间。在最佳糖化工艺条件下,还原糖收率为3.17%。     

Preparation of microcrystalline cellulose from rice straw under microwave irradiation

Crude cellulose was isolated from rice straw and then converted into microcrystalline cellulose (MCC) via partial hydrolysis. Both the isolation and partial hydrolysis were carried out under microwave. Rice straw was successively pretreated with alkaline and acid solutions before hydrolysis. Lignin and silica were almost removed but partial removal of hemicellulose in dilute alkali solution, and the residual hemicellulose was further removed in dilute acid solution. The total removal rates of hemicellulose, lignin and silica reached up 92.0%, 98.5%, and 96.8%, respectively. The cellulose content of 93.6 wt % in MCC was given by partial hydrolysis of crude cellulose isolated from rice straw. The comparison between microwave irradiation and traditional heating method was also investigated. Compared to traditional heating method, similar results were obtained while milder conditions, including shorter time and lower temperature, were required. An effective microwave‐assisted and energy‐efficient methodology using rice straw as the alternative source of cellulose fiber was developed. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44901.     

树脂型固体酸催化水解稻草秸秆的新工艺研究

对利用树脂型固体酸催化剂催化水解稻草秸秆制备可溶性糖工艺进行了研究,单因素考察了固固比、固液比、反应温度、反应时间、秸秆目数对秸秆水解产率的影响。研究结果表明:秸秆粉碎至100目,常压下固液比(反应体系中固形物与液体质量比)为1∶10、固固比(树脂型固体酸与秸秆质量比)为1∶1、反应温度100℃、反应时间15 h为最适反应条件,在该条件下树脂型固体酸催化水解稻草秸秆反应的水解产率为32.5%。该新工艺为稻草秸秆的水解利用开辟了一条绿色环保的新途径。     

Evaluation of enzymatic hydrolysis of wheat straw pretreated by atmospheric glycerol autocatalysis

BACKGROUND: Because ethanol organosolv pulping requires high pressure and is highly volatile, an atmospheric autocatalytic glycerol organosolv pretreatment process has been investigated. Enzymatic hydrolysis of wheat straw pretreated using this method was evaluated to explore a novel, economically competitive and environmentally friendly pretreatment technology for bioconversion of lignocellulosic biomass. The method also provides economical utilization of industrial glycerol, helping to cope with the challenge of the excess production of glycerol and to further defray the cost of biodiesel production. RESULTS: With preliminary optimization of the parameters in the pretreatment process, pretreatment performed at 240 °C for 4 h with the glycerol addition of 15 g g^?1 dry feedstock and wash at 80 °C led to high recovery of cellulose (95%) and good removal of lignin (>70%), which formed, respectively, 80% and 10% of the pulp. The enzymatic hydrolysis of the pretreated wheat straw yielded 90% of theoretically achievable sugar after 24 h and 92% after 48 h. CONCLUSION: Atmospheric autocatalytic glycerol organosolv pretreatment removed significant amounts of hemicellulose and lignin without affecting good cellulose recovery. The proposed novel strategy increased the susceptible of wheat straw to enzyme attack and led to enzymatic hydrolysis that was comparable with that achieved using ethanol organosolv pretreatment. Copyright © 2007 Society of Chemical Industry     

Microwave-assisted catalyst-free hydrolysis of fibrous cellulose for deriving sugars and biochemicals

Microwave (MW) assisted catalyst-free hydrolysis of fibrous cellulose (FC, cellulolysis) at 200°C promoted a cellulose conversion of ca. 37.2% and quantitative production of valuable C5/C6 sugars (e.g., glucose) and the according platform biochemicals (e.g., 5-hydroxymethylfurfural), corresponding to an overall selectivity of 96.5%. Conversely, conventional hydrothermal cellulolysis under similar conditions was not effective, even after 24 h, carbonising the FC. Based on the systematic study of MW-assisted cellulolysis, the specific interaction between water molecules and macroscopic FC under the MW irradiation was proposed, accounting for the interpretation of the experimental observation. The kinetic energy of water molecules under the MW irradiation facilitated the C–C (in the non-hindered surface –CH₂OH groups) and C–O–C bond breaking (inside the cellulose cavities) in FC, producing primary cellulolysis products of xylose, glucose and cellobiose.     

微晶纤维素超临界水解糖化的研究

于420℃的盐浴温度下,在80 g水中分别加入1～5 g的微晶纤维素,进行了纤维素超临界水解产糖的研究.结果表明随着固液比的增大,还原糖和己糖含量均升高,但液化率下降,最大还原糖质量浓度为13.05 g/L,对应的己糖质量浓度为7.12 g/L,液化率50.6%,己糖产率为11.4%,电镜图片显示水解残渣的表面有大量的孔洞,同时形成了大量的球状颗粒.     

秸秆醋酸纤维素的制备

农作物秸秆是自然界中数量极大的可再生资源,本研究以农作物秸秆为反应原料,采用无污染蒸汽爆破技术活化预处理,然后进行乙酰化反应,通过溶剂萃取分离并制备出高附加值的醋酸纤维素。实验结果表明：秸秆汽爆后明显增加了反应活性,制备醋酸纤维素的适宜条件是123℃,2 h,催化剂用量为7％,汽爆秸秆中性洗涤剂处理后的乙酰化结果效果最好,不同汽爆秸秆中小麦秸秆乙酰化效果最佳,优化实验条件下,秸秆醋酸纤维素聚合度均在120以上,取代度2.80以上,并且用红外图谱、1H NMR进行了表征。与目前工业上采用α-纤维素含量较高的高级浆为反应原料相比,不仅原料和预处理成本大大降低,而且工艺流程简单。     

Acid hydrolysis behaviour of microbial cellulose II

A mutant strain of Acetobacter xylinum produces cellulose of anomalous band-like form (‘native band’), and this material has been found to be cellulose II, presumably having a folded-chain structure (according to recent work by Kuga et al.). In addition to the previous results of electron diffraction, X-ray analysis showed that this band material was composed of virtually pure cellulose II. We have studied the acid hydrolysis behaviour of this material to obtain additional evidence for the proposed structure. When hydrolysed with 1 N hydrochloric acid at 100°C, the degree of polymerization (DP) of the material decreased rapidly from 322 ( ) to 18.3 ( ). The latter value (levelling-off DP) corresponds to the observed width (10 nm) of strand-like constituents of the band material. The sample dissolved in and regenerated from 8.75% aqueous sodium hydroxide lost its original characteristic morphology and became irregular-shaped agglomerates. The leveling-off DP of this regenerated sample was 55.2 ( ), a typical value for common regenerated celluloses. These findings as a whole strongly suggest that the cellulose molecules in the native band are selectively cleaved at sharply folded parts by acid, producing fragments of the length of folding periodicity.