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MOLECULES · 2023 ·Vol. 28 ·期 8 ·3616 · IF 4.6

Optimization of Physical Refining Process of Camellia Oil for Reduction of 3-Monochloropropane-1,2-Diol (3-MCPD) Ester Formation Using Response Surface Methodology on a Laboratory Scale

Liqun Zhang,Pinggu Wu,Xiaoling Xiang,Dajin Yang,Liyuan Wang,Zhengyan Hu

Refined and deodorized camellia oil has been reported to contain a high amount of 3-monochloropropane-1,2-diol esters (3-MCPDE) due to the high-temperature deodorization step. To reduce 3-MCPDE in camellia oil, the physical refining process of camellia oil was simulated on a laboratory scale. Response surface methodology (RSM) was designed to modify and optimize the refining process with five processing parameters (water degumming dosage, degumming temperature, activated clay dosage, deodorization temperature and deodorization time). The optimized new refining approach achieved a 76.9% reduction in 3-MCPDE contents, in which the degumming moisture was 2.97%, the degumming temperature was 50.5 °C, the activated clay dosage was 2.69%, the deodorizing temperature was 230 °C, and the deodorizing time was 90 min. A significance test and analysis of variance results demonstrated that the deodorization temperature and deodorization time contributed significantly to the reduction of 3-MCPD ester. The joint interaction effects of activated clay dosage and deodorization temperature were significant for 3-MCPD ester formation.Keywords:3-MCPD esters;response surface analysis;optimized refining process parameters;reduction of 3-MCPD

研究领域: 食品科学 · 化学工程
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Journal of Manufacturing Processes · 2021 · IF 5.01

Modeling of bonding strength for Fused Filament Fabrication considering bonding interface evolution and molecular diffusion

Mengyuan Zhou,Xiaowei Zhou,Liang Si,Peng Chen,Maoyuan Li,Yun Zhang,Huamin Zhou

Fused Filament Fabrication (FFF) is one of the most widely used material extrusion additive manufacturing techniques . Its application is limited by the poor mechanical properties because of the weak bonding interface between strands. Although numerous experimental studies have investigated the effects of process parameters on mechanical performances, the bonding fracture mechanism and the quantitative relationship between process parameters and the bonding strength are not well understood. Here, we report a novel theoretical model considering coupled effects of the bonding interface evolution and molecular diffusion for predicting the bonding strength, which provides a comprehensive insight into the FFF bonding process. The model establishes an accurate relationship between process parameters and the bonding strength parallel/perpendicular to the deposition direction. Predictions agree well with experimental results and the average root mean square error (RMS) is ~5.52%. The fracture mechanism confirms the variation of the bonding interface and molecular diffusion assumed in the model. The bonding interface evolution and molecular diffusion are proved to play an important role in the bonding strength.

研究领域: 材料科学 · 力学
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JOURNAL OF MEMBRANE SCIENCE · 2024 · IF 8.4

Large-scale preparation of composite membranes for CO2 separation via interfacial polymerization: Monomer selection and processing parameter optimization

Ye Yuan,Fei Shi,Qinghua Li,Yi Yang,Xiangyu Cai,Menglong Sheng,Zhi Wang

The increasingly serious situation of CO 2 emissions compels researchers to pay extensive attention to industrial processes for carbon capture. Membrane-based separation technology is widely regarded as a promising reserve method for carbon capture, featuring a wide adjustment range, flexible operation and modular design. In this work, a large-scale interfacial polymerization membrane production process for carbon capture was developed together with the construction of novel interfacial polymerization equipment with an adjustable organic phase bath and surface cross-linking unit. A monomer suitable for efficiently preparing high-performance CO 2 separation membranes was selected through a combination of experiments and simulations. The effect of production conditions on the structure and performance of large-scale membranes was investigated. The performance resilience at high pressure and short-term stability in the presence of impurities of the optimized membranes were examined. Techno-economic evaluation targeting carbon capture from post-combustion gas verifies the significant industrial application potential of the membranes.

CAS / MDL: 4422-95-1 142-82-5
研究领域: 材料科学 · 环境工程
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CONSTRUCTION AND BUILDING MATERIALS · 2023 · IF 7.4

Study on materials composition and process parameters of polyurethane-modified asphalt synthesized in-situ by the one-shot process

Tianhong Yang,Zhaoyi He,Gang Huang,Yongli Zhao,Jianwei Fu,Hao Xiang,Yingju Zhou

To improve the performance of ordinary road asphalt, and overcome the problems of poor thermal storage stability, easy segregation, and high preparation temperature of polymer-modified asphalt such as SBS (styrene–butadienestyrene block copolymer) or rubber powder. Polyurethane-modified asphalt (PUMA) was synthesized in-situ by the one-shot process with varying dosages of polyurethane (PU) raw materials (2.86 wt% ∼ 11.94 wt%) and isocyanate index R (–NCO/–OH) values (2, 3, 5, and 7) for a total of 12 samples, in this study. The material composition, development time, and modification mechanism of PUMA were analyzed using the approach of “macro performance + micro mechanism”. Firstly, the conventional properties, rotational viscosity, and rheological properties of PUMA samples were evaluated and compared to virgin asphalt. Secondly, under the optimal material composition scheme, the conventional performance and thermal storage stability differences between MOCA (3, 3′ -dichloro-4,4′ -diamino diphenyl methane) and BDO (1,4-butanediol) were compared. Comparing the performance of PUMA during the development times of 0 to 12 h, the oven temperature is 105 °C. Fourier transform infrared spectroscopy (FTIR) and fluorescence microscopy (FM) were used to analyze the chemical structure and spatial structure of PU in asphalt. The results indicate that: 1) the higher the R (–NCO/–OH), the higher the asphalt's high-temperature performance, elastic recovery performance, and viscosity, but the lower its low-temperature performance. 2) Under the same R (–NCO/–OH) condition, the increase in PU has little effect on the preceding performance. 3) MOCA is marginally superior to BDO in terms of high-temperature performance, whereas BDO has greater advantages in terms of low-temperature performance; compatibility is comparable. 4) At 105 °C, the performance continued to improve for 0 to 5 h, but after 5 to 12 h, the improvement was no longer noticeable. 5) Due to the reaction of the isocyanate group with the polyol and the active group in the asphalt, functional groups such as carbamate and urea are directly synthesized in the asphalt, allowing the PU molecular chain to expand and form a network structure within the asphalt. This procedure modifies the performance of the virgin asphalt. These findings not only improve our understanding of the effect of optimal material composition and development time on the properties of PUMA, but they also provide direction for future research.

研究领域: 材料科学 · 化学工程
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JOURNAL OF MATERIALS SCIENCE · 2025 · IF 3.9

Influence of drying process conditions on graphite anode properties and crystalline type of polyvinylidene fluoride binder

Niu Lijing,Zhao Jiajia,Xie Mengmeng,Jiang Xunyong

Dry electrode manufacturing methods that do not use NMP can reduce the time and energy required to produce lithium-ion batteries. Polyvinylidene fluoride (PVDF) is a commonly used binder in the dry process. However, there is a lack of research on the effect of dry process parameters on PVDF crystalline types. In our work, the dry process parameters of graphite anode with PVDF as binder are studied, such as the effects of temperature, pressure, and time on the crystallization of PVDF. The effects of powder mixing process and binder content on the performance of dry graphite electrodes are investigated. PVDF processed at 180 °C, 6 MPa, and for 15 min under hot pressing conditions favors the presence of β-crystalline forms. The capacity retention of the prepared electrodes with 10% PVDF loading is superior to that of conventional wet electrodes. Subsequently, reducing PVDF to 5% induces additional cycling stability and rate handling improvements of the dry electrode. Graphical abstract

CAS / MDL: 7439-93-2
研究领域: 材料科学 · 电化学
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Analytical Methods · 2015 ·Vol. 7 ·期 11 ·4616-4620 · IF 1.821

Rapid screening of critical process parameters based on near infrared spectroscopy: a case study of the ethanol precipitation process

Binjun Yan,Haibin Qu

In process development, the design of experiments (DoE) approach has been widely used for screening the key influential factors and obtaining optimal operating conditions. However, measuring the quality attributes of many products produced in the DoE is time and cost intensive. Therefore, an innovative method using near infrared spectroscopy (NIRS) for rapid screening of CPPs is proposed in this work, taking the ethanol precipitation process of Danhong Injection as a case study. In this work, seven process parameters were studied with a fractional factorial DoE. The supernatants produced were analyzed by NIRS. The spectra were preprocessed and then decomposed by principal component analysis into a few scores and loadings. The scores were taken as the response variables in analysis of variance (ANOVA) to identify the CPPs. The results showed that water content in the concentrate (p < 0.0001), ethanol concentration (p < 0.0001) and ethanol consumption (p < 0.0001) were the three CPPs. To validate the proposed method, the intermediates were analyzed by HPLC. The concentrations of two representative compounds were taken as the response variables in ANOVA and the same three CPPs were identified. The proposed method was successfully applied and the advantages of integrating spectroscopic techniques into screening DoE were demonstrated.

CAS / MDL: 78281-02-4
研究领域: 制药工程 · 生物技术
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Foods · 2023 ·Vol. 12 ·期 5 ·975 · IF 5.2

Effects of Addition of Tea Polyphenol Palmitate and Process Parameters on the Preparation of High-Purity EPA Ethyl Ester

Xuyang Ding,Fujun Liu,Rui Zheng,Xuechen Pei,Ziye Wang,Dayong Zhou,Fawen Yin

High-purity eicosapentaenoic acid (EPA) ethyl ester (EPA-EE) can be produced from an integrated technique consisting of saponification, ethyl esterification, urea complexation, molecular distillation and column separation. In order to improve the purity and inhibit oxidation, tea polyphenol palmitate (TPP) was added before the procedure of ethyl esterification. Furthermore, through the optimization of process parameters, 2:1 (mass ratio of urea to fish oil, g/g), 6 h (crystallization time) and 4:1 (mass ratio of ethyl alcohol to urea, g/g) were found to be the optimum conditions in the procedure of urea complexation. Distillate (fraction collection), 115 °C (distillation temperature) and one stage (the number of stages) were found to be the optimum conditions for the procedure of molecular distillation. With the addition of TPP and the above optimum conditions, high-purity (96.95%) EPA-EE was finally obtained after column separation.

研究领域: 食品科学 · 生物化学
✓ 已验证 DOI PubMed 高影响因子
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PLoS One · 2015 ·Vol. 10 ·期 5 ·e0128236 · IF 3.234

Design Space Development for the Extraction Process of Danhong Injection Using a Monte Carlo Simulation Method

Xingchu Gong,Yao Li,Huali Chen,Haibin Qu

A design space approach was applied to optimize the extraction process of Danhong injection. Dry matter yield and the yields of five active ingredients were selected as process critical quality attributes (CQAs). Extraction number, extraction time, and the mass ratio of water and material (W/M ratio) were selected as critical process parameters (CPPs). Quadratic models between CPPs and CQAs were developed with determination coefficients higher than 0.94. Active ingredient yields and dry matter yield increased as the extraction number increased. Monte-Carlo simulation with models established using a stepwise regression method was applied to calculate the probability-based design space. Step length showed little effect on the calculation results. Higher simulation number led to results with lower dispersion. Data generated in a Monte Carlo simulation following a normal distribution led to a design space with a smaller size. An optimized calculation condition was obtained with 10000 simulation times, 0.01 calculation step length, a significance level value of 0.35 for adding or removing terms in a stepwise regression, and a normal distribution for data generation. The design space with a probability higher than 0.95 to attain the CQA criteria was calculated and verified successfully. Normal operating ranges of 8.2-10 g/g of W/M ratio, 1.25-1.63 h of extraction time, and two extractions were recommended. The optimized calculation conditions can conveniently be used in design space development for other pharmaceutical processes.

研究领域: 中药学 · 制药工程
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Materials · 2021 ·Vol. 14 ·期 5 ·1100 · IF 3.623

Influence of Sintering Process Conditions on Microstructural and Mechanical Properties of Boron Carbide Ceramics Synthesized by Spark Plasma Sintering

Yingying Liu,Sheng Ge,Yihua Huang,Zhengren Huang,Deku Zhang

Boron carbide (B4C) ceramics were synthesized by spark plasma sintering at a temperature between 1600 and 2050 °C without employing any sintering additives. The effect of sintering process parameters, such as temperature, holding time, pressure, hearting rate, and pulsed electric current, and the particle size of the raw powder on the densification behavior and mechanical properties of B4C ceramics, were comprehensively and systematically investigated. Hardness and fracture toughness of B4C that has a density close to the theoretical value were found to be 33.5 ± 0.2 GPa and 3.21 ± 0.13 MPa·m1/2, respectively. Electron backscatter diffraction (EBSD) analysis revealed no abnormal growth of grains due to an increase in holding time and pressure. Twin structures present in ceramics are beneficial for their mechanical performance.

研究领域: 材料科学 · 机械工程
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International Journal of Bioprinting · 2017 ·Vol. 3 ·期 1 ·009 · IF 0

Influence of electrohydrodynamic jetting parameters on the morphology of PCL scaffolds

Hang Liu,Sanjairaj Vijayavenkataraman,Dandan Wang,Linzhi Jing,Jie Sun,Kai He

One of the important constituents in tissue engineering is scaffold, which provides structural support and suitable microenvironment for the cell attachment, growth and proliferation. To fabricate micro/nano structures for soft tissue repair and three-dimensional (3D) cell culture, the key is to improve fibre-based scaffold fabrication. Electrohydrodynamic (EHD) jetting is capable of producing and orientating submicron fibres for 3D scaffold fabrication. In this work, an EHD-jetting system was developed to explore the relationship between vital processing parameters and fibre characteristics. In this study, polycaprolactone (PCL) solution prepared by dissolving PCL pellets in acetic acid was used to fabricate the scaffolds. The influence of voltage, motorized stage speed, solution feed rate, and solution concentration on fibre characteristics and scaffold pattern were studied. Morphology of the EHD-jetted PCL fibres and scaffolds were analysed using optical microscope images and scanning electron microscope (SEM) images. Multi-layer scaffolds with the varied coiled pattern were fabricated and analysed. Cell attachment and proliferation have to be investigated in the future by further cell culture studies on these multi-layer coiled scaffolds.

研究领域: 生物材料 · 组织工程 · 高分子科学 · 再生医学 · 生物制造
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Chinese Herbal Medicines · 2019 · IF 0

Critical process parameter identification of manufacturing processes of Astragali Radix extract with a weighted determination coefficient method

Min-fei Sun,Jing-yi Yang,Wen Cao,Jing-yuan Shao,Guo-xiang Wang,Hai-bin Qu,Wen-hua Huang,Xing-chu Gong

Objective Critical process parameters (CPPs) identification is an important step of the implementation of quality by design (QbD) concept. There are many CPP identification methods, such as risk analysis method, sensitivity analysis method, multiple linear regression method, standard partial regression coefficient (SPRC) method, and so on. The SPRC method can consider multiple process critical quality attributes (CQAs) simultaneously, but the determination of CPP number is subjective. Therefore, new CPP identification method is still required. Methods The manufacturing process of Astragali Radix extract, which contained water reflux extraction, concentration, and ethanol precipitation, was used as an example. First, the multiple process CQAs were determined to be the yield of pigment, dry matter, sugars, and active ingredients. Second, the potential CPPs were determined by a knowledge organization method. Plackett-Burman designed experiments were then performed. A weighted determination coefficient ( R w 2 Rw2 ) method was presented to identify CPPs. In this method, the importance of different CQAs was considered. Process parameters were removed one-by-one according to their importance index. The decrease in R w 2 Rw2 was used to characterize the importance of the removed parameter. If the decrease of R w 2 Rw2 was less than a preset threshold, the removed parameter was not a CPP. Results During the manufacturing process of Astragali Radix extract, the potential CPPs determined by the knowledge organization method were water consumption, reflux extraction time, extraction frequency, ethanol content, ethanol consumption, and concentration endpoint. Reflux extraction time, the first ethanol consumption, the second ethanol consumption, and the second ethanol precipitation refrigeration temperature were found to be CPPs using the weighted determination coefficient method with the threshold of 10%. Conclusion Using the weighted determination coefficient method, CPPs can be determined with all the CQAs considered based on their importance. The determination of CPP number is more objective compared with the SPRC method.

CAS / MDL: 57-48-7 121-44-8
研究领域: 中药学 · 制药工程
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JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY · 2023 ·Vol. 107 ·期 2 ·490-502 · IF 2.5

Optimization of the sol gel synthesis process parameters by orthogonal experiment of novel spinel oxide catalyst CuFe1.2Al0.8O4 with improved performance for methanol steam reforming

Shen Qiuwan,Cai Zhongwen,Chen Gaokui,Zhang Xin,Li Shian,Yang Guogang

In this study, optimization of the synthesis process parameters of sol-gel method using orthogonal experiment was first applied for CuFe 1.2 Al 0.8 O 4 catalysts in methanol steam reforming (MSR). OA 9 (4 4 ) orthogonal experiments were applied to optimize the synthesis process parameters by sol-gel method, including precursor copper source complexing agent, calcination temperature, and calcination time. The MSR performance was selected as the objective function. Results show that copper source has the greatest impact among the four factors on the catalytic performance. The catalytic performance of the catalyst synthesized by using copper hydroxide as the precursor copper source was much better than the other copper sources. For the other three factors, the order of important factors is: calcination time > complexing agent > calcination temperature. According to the results of range analysis, the optimal synthesis process parameters for CuFe 1.2 Al 0.8 O 4 with best MSR performance are as follows: the precursor copper source is copper hydroxide, the calcination time is 2 h, the complexing agent is ethanol and ethylene glycol, and the calcination temperature is 700 °C. The hydrogen production is 0.077 mol/min/g oat , the methanol conversion rate can reach >95%, and the hydrogen selectivity can reach 99%. CuFe 1.2 Al 0.8 O 4 spinel oxide catalyst which synthesized in this study has excellent catalytic performance for hydrogen production in MSR. Its low CO selectivity makes it a potential catalyst for producing high-purity hydrogen. Graphical Optimization of the synthesis process parameters of sol-gel method using orthogonal experiment was first applied for CuFe 1.2 Al 0.8 O 4 catalysts in methanol steam reforming (MSR). Its low CO selectivity makes it a potential catalyst for producing high-purity hydrogen.

研究领域: 材料科学 · 催化化学 · 能源化学 · 化学工程 · 纳米技术
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