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Abstract ：
In the burgeoning sucralose (TGS) production, the separation bottleneck has hindered its further technology upgrading. In this work, the crystal structural of sucrose-6-acetate chlorination product 4,1 ',6 '-trichlorosucrose-6- acetate hydrate (TSA-6.2H2O) from multi-step recrystallization has been determined, thus the bad separation efficiency of the chlorination process was assigned to the easy incorporation of by-products into the cavities or local defects of the respirable TSA-6.2H2O network. Based on this mechanism, the second cheap organic solvents have been pre-embedded into TSA-6.2H2O to generate stable ternary solvates, i. e. TSA-6.H2Osecond solvent (second solvent = DMF (N,N'-dimethylformamide), DMAc (N, N'-dimethylacetamide), and NMP (N-methyl-2pyrrolidone)). Their cellular-type compacted arrangements were constructed from strong hydrogen bonding interactions between H2O.second solvent guests and TSA-6 networks. Consequently, the free space or local defects for the encapsulation of impurities could be inhibited completely. Upon the optimization of the crystallized process (H2O: NMP = 7: 3, solvent: TSA-6 = 12: 1, operating temperature: 288.2 K), high TSA-6 purity (99.74 % wt) and low sum of alpha x (0.023) can be achieved. Furthermore, under the guidance of ternary phase diagrams (TPD), the second solvents could be facilely removed by modulating the H2O/second solvent ratio (TSA-6 purity: 99.91 % wt in 0.5 h). In all, the clarification on the obscure mechanism and the strategy of pre-embedding second solvents have broken the separation bottleneck in TGS production, which can also be applied in other relative glycosyl halides industries.
Keyword ：
1 ' 1 ' 6 ' -trichlorosucrose-6-acetate 6 ' -trichlorosucrose-6-acetate Hydrogen bond framework Hydrogen bond framework Selective separation by solvation-induced Selective separation by solvation-induced Separation mechanism Separation mechanism Ternary phase diagrams Ternary phase diagrams
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| GB/T 7714 | Chen, Xiaoping , Lei, Jiayan , Lv, Zhoulin et al. Breaking separation bottleneck in sucralose production: Clarifying the obscure mechanism and pre-embedding second solvents for highly selective separation of chlorinated product [J]. | CHEMICAL ENGINEERING JOURNAL , 2025 , 504 . |
| MLA | Chen, Xiaoping et al. "Breaking separation bottleneck in sucralose production: Clarifying the obscure mechanism and pre-embedding second solvents for highly selective separation of chlorinated product" . | CHEMICAL ENGINEERING JOURNAL 504 (2025) . |
| APA | Chen, Xiaoping , Lei, Jiayan , Lv, Zhoulin , Chen, Zi'ang , Lin, Shitong , Guo, Zhenming et al. Breaking separation bottleneck in sucralose production: Clarifying the obscure mechanism and pre-embedding second solvents for highly selective separation of chlorinated product . | CHEMICAL ENGINEERING JOURNAL , 2025 , 504 . |
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Lithium bis(fluorosulfonyl)imide (LiFSI) is a promising electrolyte for lithium-ion batteries. However, the lithiation reaction during the LiFSI synthesis process is accompanied by a LiFSI hydrolysis reaction, which negatively affects the LiFSI yield and poses potential safety risks. In this study, we delve into the reaction equilibrium and hydrolysis behavior during the lithiation reaction and identify that the high temperature and strong alkali used in the reactive distillation process are the key factors leading to LiFSI hydrolysis. As a solution, a novel method for effectively synthesizing LiFSI using reaction-extraction coupling method is proposed and rigorously tested for various factors, including temperature, alkali equivalent, type of solvent, and dosage. The research culminated in developing a multistage continuous membrane extraction process, which achieves a remarkable conversion of over 99.7 % and minimizes LiFSI hydrolysis to less than 0.05 %.
Keyword ：
Hydrolysis Hydrolysis LiFSI LiFSI Lithiation Lithiation Reaction-extraction coupling method Reaction-extraction coupling method Sequential synthesis Sequential synthesis
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| GB/T 7714 | Zhou, Shouquan , Liu, Yan , Ren, Fengjiao et al. Efficient synthesis of LiFSI based on Reaction-Extraction coupling method [J]. | SEPARATION AND PURIFICATION TECHNOLOGY , 2025 , 362 . |
| MLA | Zhou, Shouquan et al. "Efficient synthesis of LiFSI based on Reaction-Extraction coupling method" . | SEPARATION AND PURIFICATION TECHNOLOGY 362 (2025) . |
| APA | Zhou, Shouquan , Liu, Yan , Ren, Fengjiao , Zhang, Siyu , Shi, Xueying , Wu, Bin et al. Efficient synthesis of LiFSI based on Reaction-Extraction coupling method . | SEPARATION AND PURIFICATION TECHNOLOGY , 2025 , 362 . |
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Dehydroxylation of biomass-based platform molecules is critical for obtaining building blocks for use in the chemical industry. Acid catalytic dehydration has provided a feasible route. However, simultaneously pursuing high product-selective and ultra-stable catalysts for the dehydroxylation of polyols remains an open challenge. In this study, a strategy for in-situ Bronsted acid sites (BAS) with chemo-adsorption selectivity is proposed. The construction of defect sites B[3] and P[4] species has been proved to be a prerequisite for the dynamic acid site formation at hydrothermal conditions. The BPO4 catalyst with in-situ BAS can achieve the high selectivity of acrolein (similar to 80%) and robust stability of catalyst (over 425 h) using glycerol dehydration as a model reaction. In addition, in-situ BAS is highly selective for secondary hydroxyl groups and has been extended to other substrate applications. This catalytic strategy provides a green, efficient, and economical approach for converting biomassderived polyols to high-value-added chemicals.
Keyword ：
Acrolein Acrolein Biomass Biomass Dehydration Dehydration Glycerol Glycerol In -situ Br onsted acid In -situ Br onsted acid
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| GB/T 7714 | Su, Chenxin , Zhou, Shouquan , Wu, Shaoyun et al. Highly efficient dehydration of polyols: In-situ Brempty setnsted acid from boron phosphate catalyst [J]. | CHEMICAL ENGINEERING JOURNAL , 2024 , 483 . |
| MLA | Su, Chenxin et al. "Highly efficient dehydration of polyols: In-situ Brempty setnsted acid from boron phosphate catalyst" . | CHEMICAL ENGINEERING JOURNAL 483 (2024) . |
| APA | Su, Chenxin , Zhou, Shouquan , Wu, Shaoyun , Gao, Mingbin , Zhang, Weiling , Ma, Zhuang et al. Highly efficient dehydration of polyols: In-situ Brempty setnsted acid from boron phosphate catalyst . | CHEMICAL ENGINEERING JOURNAL , 2024 , 483 . |
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The Microscale Oscillatory Flow Reactor (MOFR) can achieve good plug flow and micromixing performance simultaneously at laminar net flow conditions. An unbaffled U-shaped microreactor coupled with oscillating flow technology was designed to study the macro and micromixing performance. Firstly, the influence of oscillations on the flow performance was studied to reveal the formation rule of vortex. The simulation results showed that the continuous formation and destruction of periodic vortexes occurred in the microreactor with oscillation. With the increase of oscillation intensity, the vortex size in the radial direction first gradually increased and then becomes stable, and gradually moved axially, resulting in axial diffusion. Secondly, the effect of oscillation on the macromixing and micromixing performance were investigated. The results showed that the coupling oscillation could greatly improve the macromixing and micromixing performance. The macromixing and micromixing performance were promoted simultaneously at lower oscillation intensity and then tended to be flat due to the axial diffusion at high oscillation intensity. When phi>6.05, the minimum micromixing time and the maximum number of tanks can be achieved at the same time. At a velocity ratio of about 23, FoM reached a maximum of about 3.5.
Keyword ：
CFD CFD Macromixing Macromixing Micromixing Micromixing MOFR MOFR Vortex Vortex
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| GB/T 7714 | Yu, Liping , Zheng, Meiqin , Wang, Jiawei et al. Enhanced mixing characteristics of unbaffled U-shaped microreactor coupled oscillatory flow [J]. | CHEMICAL ENGINEERING AND PROCESSING-PROCESS INTENSIFICATION , 2024 , 205 . |
| MLA | Yu, Liping et al. "Enhanced mixing characteristics of unbaffled U-shaped microreactor coupled oscillatory flow" . | CHEMICAL ENGINEERING AND PROCESSING-PROCESS INTENSIFICATION 205 (2024) . |
| APA | Yu, Liping , Zheng, Meiqin , Wang, Jiawei , Yan, Zuoyi , Yao, Wei , Li, Haohong et al. Enhanced mixing characteristics of unbaffled U-shaped microreactor coupled oscillatory flow . | CHEMICAL ENGINEERING AND PROCESSING-PROCESS INTENSIFICATION , 2024 , 205 . |
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本发明提供了一种三氯蔗糖‑6‑乙酸酯生产工艺：向一次蒸馏得到的蔗糖乙酸酯浓缩液中加入冰醋酸与第一有机溶剂混合溶液，得到蔗糖‑6‑乙酸酯与乙酸的白色共晶体粉末；将共结晶体均匀分散在第二有机溶剂中，加入有机胺处理，使之与乙酸反应形成稳定的化学键，从共晶体骨架中夺取乙酸，对于残留的有机胺以及形成的乙酸‑有机胺结合物使用第二有机溶剂洗涤，烘干完全后获得大于99.8%的蔗糖‑6‑乙酸酯粉末；并将该粉末溶解于N, N‑二甲基甲酰胺溶液中，应用于下一步区域选择性氯代反应，消除了杂质对氯代反应过程的不良影响，提升了氯代收率，简化了三氯蔗糖‑6‑乙酸酯提纯过程，提高了最终三氯蔗糖的产品品质，具有更好的工业价值。
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| GB/T 7714 | 郑辉东 , 陈小平 , 陈子昂 et al. 一种三氯蔗糖-6-乙酸酯生产工艺 : CN202210020727.0[P]. | 2022-01-10 00:00:00 . |
| MLA | 郑辉东 et al. "一种三氯蔗糖-6-乙酸酯生产工艺" : CN202210020727.0. | 2022-01-10 00:00:00 . |
| APA | 郑辉东 , 陈小平 , 陈子昂 , 陈晶晶 , 林诗童 , 李少恒 et al. 一种三氯蔗糖-6-乙酸酯生产工艺 : CN202210020727.0. | 2022-01-10 00:00:00 . |
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Abstract ：
本发明公开了一种甘油脱水催化剂及其制备方法和应用，该方法通过浸渍法制备了一种负载型磷酸硼催化剂。在固定床反应器中，反应温度为280~360℃，10%~30%的甘油水溶液为原料，以该催化剂催化甘油脱水反应，甘油转化率100%，丙烯醛选择性可达76%，羟基丙酮选择性达15%。并且该催化剂具有良好的稳定性，可以反应200h未明显失活。并且经过简单再生处理，可快速恢复催化剂活性。本发明提供的催化剂，制备工艺简单，易于工业化，为生物甘油转化为高附加值产品提供了一条良好的道路。
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| GB/T 7714 | 郑辉东 , 苏晨欣 , 周守泉 et al. 一种甘油脱水催化剂及其制备方法和应用 : CN202210060922.6[P]. | 2022-01-19 00:00:00 . |
| MLA | 郑辉东 et al. "一种甘油脱水催化剂及其制备方法和应用" : CN202210060922.6. | 2022-01-19 00:00:00 . |
| APA | 郑辉东 , 苏晨欣 , 周守泉 , 吴乃昕 , 刘杰 , 陈晶晶 . 一种甘油脱水催化剂及其制备方法和应用 : CN202210060922.6. | 2022-01-19 00:00:00 . |
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本发明提供了一种蔗糖‑6‑乙酸酯脱酸提纯的方法，包括如下步骤：将蔗糖和醋酐酯化反应后生成的蔗糖‑6‑乙酸酯反应液输送至精馏塔中精馏浓缩，塔顶得到不含乙酸的DMF和水，塔底得到蔗糖‑6‑乙酸酯的浓缩液。向浓缩液中加入共晶溶剂，得到蔗糖‑6‑乙酸酯与乙酸的共晶体。将提纯后的蔗糖‑6‑乙酸酯共晶体固体用DMF进行溶解，再利用支撑液膜对蔗糖‑6‑乙酸酯溶液中的乙酸进行萃取，从而得到不含乙酸的高纯度蔗糖‑6‑乙酸酯，同时利用反萃取剂进行反萃，得到乙酸盐副产品。本发明完美解决了酯化反应液乙酸难脱除以及蔗糖‑6‑乙酸酯难提纯的问题，具有更高的工业运用价值。
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| GB/T 7714 | 揭会民 , 郑辉东 , 李浩宏 et al. 一种蔗糖-6-乙酸酯脱酸提纯的方法 : CN202310187287.2[P]. | 2023-03-02 00:00:00 . |
| MLA | 揭会民 et al. "一种蔗糖-6-乙酸酯脱酸提纯的方法" : CN202310187287.2. | 2023-03-02 00:00:00 . |
| APA | 揭会民 , 郑辉东 , 李浩宏 , 陈小平 , 陈晶晶 , 王莹淑 et al. 一种蔗糖-6-乙酸酯脱酸提纯的方法 : CN202310187287.2. | 2023-03-02 00:00:00 . |
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Sustainable synthesis of acrolein, a key chemical intermediate, from biomass-derived glycerol is highly attractive. However, conventional catalysts for the dehydration of glycerol suffer from low acrolein selectivity and high deactivation tendency. Herein, a novel green catalyst (HPW/T-0.6 S-COOH) was prepared and employed in the dehydration of glycerol in a continuous flow reactor. The performance of different catalysts and the effects of reaction conditions (reaction temperature, N-2 flow rate, and glycerol concentration) were examined. The HPW/T-0.6 S-COOH catalyst provides the best glycerol conversion of 96.38% and acrolein selectivity of 92.01%. The NH3-TPD and pyridine-FTIR results indicate that the Bronsted acid site is more susceptible to acrolein, while the weak strength acid site effectively prevents the further reaction of acrolein, providing practical insights for the rational design of efficient and continuous synthesis of acrolein catalysts.
Keyword ：
Acrolein Acrolein Continuous synthesis Continuous synthesis glycerol dehydration glycerol dehydration HPW/T0.6S-COOH catalyst HPW/T0.6S-COOH catalyst
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| GB/T 7714 | Su, Chen-Xin , Chen, Jing-Jing , Wu, Shao-Yun et al. Continuous dehydration of glycerol to Acrolein based on HPW/TS-COOH catalyzation [J]. | JOURNAL OF FLOW CHEMISTRY , 2023 , 13 (2) : 143-154 . |
| MLA | Su, Chen-Xin et al. "Continuous dehydration of glycerol to Acrolein based on HPW/TS-COOH catalyzation" . | JOURNAL OF FLOW CHEMISTRY 13 . 2 (2023) : 143-154 . |
| APA | Su, Chen-Xin , Chen, Jing-Jing , Wu, Shao-Yun , Li, Shao-Heng , Zhou, Shou-Quan , Zheng, Hui-Dong et al. Continuous dehydration of glycerol to Acrolein based on HPW/TS-COOH catalyzation . | JOURNAL OF FLOW CHEMISTRY , 2023 , 13 (2) , 143-154 . |
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Catalytic epoxidation of alkenes is an important type of organic reaction in chemical industry, and the deep insight into catalyst deactivation will help to develop new epoxidation process. In this work, series of quaternary ammoniums bearing different cationic sizes, i.e. MTOA' (methyltrioctylammonium, [(C8H17)3CH3N]'), HTMA'(hexadecyltrimethylammonium, [(C16H33)(CH3)3N]') and DMDOA' (dimethyl-dioctadecylammonium, [(C18H37)2(CH3)2N]') were incorporated with polyoxometalate (POM) anions to prepare phase transfer catalysts (PTCs), which were used in the styrene epoxidations. Among them, (MTOA)3PW4O24 exhibits the best catalytic performance judged from the highest styrene conversion rate (52%) and styrene oxide selectivity (93%), during which the styrene epoxidation conditions were opti-mized. Meanwhile, the deactivation mechanism of this kind of PTCs was proposed firstly, i.e. in the case of low H2O2 content, the oxidant can only be used in the styrene epoxidation, in which the catalyst can transform into stable Keggin-type POM. But when the content of H2O2 is higher, the excess H2O2 can re-activate the Keggin-type POM into active (PW4O24)3-anions, which can trigger the ring-opening poly-merization of styrene oxide. Consequently, the catalyst is deactivated by adhered poly(styrene oxide) irreversibly, which was determined by NMR spectra. In this situation, the active moiety {PO4[WO (O2)2]4}3-in phase-transfer catalytic system can break into some unidentified species with low W/P ratio with the presence of epoxides. This work will be beneficial for the design of new PTCs in alkene epoxi-dation in fine chemical industry.(c) 2022 The Chemical Industry and Engineering Society of China, and Chemical Industry Press Co., Ltd. All rights reserved.
Keyword ：
Catalyst deactivation mechanism Catalyst deactivation mechanism Cation size effect Cation size effect Phosphotungstic acid phase-transfer catalyst Phosphotungstic acid phase-transfer catalyst Styrene epoxidation Styrene epoxidation
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| GB/T 7714 | Xiao, Qiongna , Jiang, Yuyan , Yuan, Weiqiang et al. Styrene epoxidation catalyzed by polyoxometalate/quaternary ammonium phase transfer catalysts: The effect of cation size and catalyst deactivation mechanism [J]. | CHINESE JOURNAL OF CHEMICAL ENGINEERING , 2023 , 55 : 192-201 . |
| MLA | Xiao, Qiongna et al. "Styrene epoxidation catalyzed by polyoxometalate/quaternary ammonium phase transfer catalysts: The effect of cation size and catalyst deactivation mechanism" . | CHINESE JOURNAL OF CHEMICAL ENGINEERING 55 (2023) : 192-201 . |
| APA | Xiao, Qiongna , Jiang, Yuyan , Yuan, Weiqiang , Chen, Jingjing , Li, Haohong , Zheng, Huidong . Styrene epoxidation catalyzed by polyoxometalate/quaternary ammonium phase transfer catalysts: The effect of cation size and catalyst deactivation mechanism . | CHINESE JOURNAL OF CHEMICAL ENGINEERING , 2023 , 55 , 192-201 . |
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The mild alkali-treated 13X was employed in the liquid phase isomerization reaction of alpha-pinene to increase the yield of limonene. A maximum alpha-pinene conversion of 100% and limonene yield of 59.1% could be achieved. Crystallinity could be well retained, and the amounts of medium-strong acid sites and the distribution of Bronsted and Lewis acid sites could be changed after the mild alkali treatment for 13X zeolite. Samples with higher micropore specific surface area were easier to obtain higher yields of limonene due to shape-selectivity. A proper amount of the medium-strong acid and the synergistic effect of Bronsted and Lewis acid sites were beneficial to enhance the catalytic activity and the yield of monocyclic product limonene. The main reason for catalyst deactivation could be the decrease in the active sites due to soft coke deposition. For the regeneration process, the conversions of alpha-pinene were between 95% and 99% during the first seven cycles and the conversion dropped to 90.6% after the eighth cycle, which demonstrated that the ethanol flushing and calcination could be an effective regeneration method for the 13X catalyst used in the alpha-pinene isomerization reaction.
Keyword ：
13X zeolite 13X zeolite Limonene Limonene Mild alkali treatment Mild alkali treatment ?-pinene isomerization ?-pinene isomerization
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| GB/T 7714 | Su, Chenxin , Luo, Xiheng , Chen, Jingjing et al. Effective synthesis of limonene over mild alkali-modified 13X catalysts in alpha-pinene isomerization [J]. | MICROPOROUS AND MESOPOROUS MATERIALS , 2023 , 348 . |
| MLA | Su, Chenxin et al. "Effective synthesis of limonene over mild alkali-modified 13X catalysts in alpha-pinene isomerization" . | MICROPOROUS AND MESOPOROUS MATERIALS 348 (2023) . |
| APA | Su, Chenxin , Luo, Xiheng , Chen, Jingjing , Wu, Dan , Fan, Lihai , Liu, Jie et al. Effective synthesis of limonene over mild alkali-modified 13X catalysts in alpha-pinene isomerization . | MICROPOROUS AND MESOPOROUS MATERIALS , 2023 , 348 . |
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