微通道中合成环氧脂肪酸甲酯

采用盐酸H2O2/HCOOH法,在微通道反应器内对不饱和脂肪酸甲酯进行环氧化反应。考察了双氧水用量、甲酸用量、反应温度及催化剂用量对反应的影响,得到最优的反应条件为:m(脂肪酸甲酯):m(甲酸):m(双氧水)=1:1.5:2,反应温度40℃,催化剂浓盐酸质量分数为3%(即浓盐酸质量占原料脂肪酸甲酯质量的百分数,下同),反应时间为110 s。在该条件下,产品环氧值为4.32%。     

响应面优化法研究果糖苯酚树脂胶黏剂的合成

以果糖代替甲醛,在碱性条件下合成了果糖苯酚树脂胶黏剂。用响应面优化法对果糖苯酚树脂的合成条件进行了优化。以树脂黏度为考察指标,根据Box-Behnken的中心组合设计原理对实验进行设计和结果分析。用响应面优化法研究了温度、时间和催化剂用量对反应的联合影响,得出最佳工艺条件为:反应温度72.36℃,反应时间6.96h,催化剂用量7.98%。在此条件下,树脂的黏度为27.67s。同时用红外光谱(IR)对树脂结构进行了分析。     

Proton Nuclear Magnetic Resonance-Based Method for the Quantification of Epoxidized Methyl Oleate

Epoxidized methyl esters (EMO) with their high oxirane ring reactivity, acts as a raw material in the synthesis of various industrial chemicals including polymers, stabilizers, plasticizers, glycols, polyols, carbonyl compounds, biolubricants etc. EMO has been generally quantified by the gas chromatography (GC) and high-performance liquid chromatography (HPLC) techniques. Taking into the account of the limitations of these techniques, two qHNMR-based equations have been proposed for the quantification of EMO in the mixture of EMO and methylesters (MO). The validity of the proposed method was determined using standard mixtures of MO and EMO having different molar concentrations. The developed equations have been applied on the samples of EMO prepared from oleic acid in two-step process viz., esterification followed by epoxidation. The qHNMR-based EMO quantification showed acceptable agreement with the results obtained from HPLC analysis.     

Optimization of Selective Lipase-Catalyzed Feruloylated Monoacylglycerols by Response Surface Methodology

The use of solvent engineering to achieve selective enzymatic synthesis of feruloylated acylglycerols during the transesterification of ethyl ferulate with TAG was investigated. Novozym 435 catalyzed transesterification of ethyl ferulate and TAG resulted in a mixture of feruloylated monoacylglycerols (FMAG) and feruloylated diacylglycerols (FDAG). These feruloylated acylglycerols have recently received much attention because of their health benefits, antioxidant properties and UV absorption. However, FMAG in a pure form is more advantageous than the FMAG–FDAG mixture in exhibiting stabilizing, emulsifying and conditioning properties. Thus, it is significant to perform efficient selectivity in the synthetic process. In this present study, the effect of various solvent mixtures, including unitary, binary and ternary organic media selective enzymatic synthesis of feruloylated acylglycerols was investigated by response surface methodology. Selectivity towards FMAG substantially increased from 14.5% in the unitary solvent n-hexane to 94.2% in the binary mixtures of 2-methyl-2-butanol (2M2B) and toluene (1:1, v/v). The maximum conversion achieved was 75.4% in this binary mixture medium. Analysis of variance (ANOVA) showed that 99.6% of the observed variation was explained by the polynomial model. Lack of fit analysis indicated that the regress equation was adequate for predicting the degree of the selectivity.     

Optimization of Vegetal Pear Drying Using Response Surface Methodology

The aim of this work was to optimize the drying process of vegetal pear and minimize energy resources (cost) under prefixed limits involving vegetal pear moisture, color, and productivity. The optimization of vegetal pear drying was made by using response surface methodology (RSM) for minimum process cost and color difference between fresh and dried samples (moisture ≤0.10 g water g d.m.^?1). A pilot-plant dryer was used for dehydrating vegetal pear slices (0.5 cm thickness). The tests were carried out at different air temperature (60 to 70°C), samples diameter (4 to 7 cm), and pretreatment with ascorbic acid solutions (0–0.1% w/w). The optimum drying conditions were found at air temperature of 63°C with 5-cm sample diameter and 0.075% of ascorbic acid concentration. On the optimized drying conditions, dried vegetal pear presented values with moisture content of 0.052 g water g d.m.^?1, color difference of 11.65, production rate of 0.0073 kg h^?1, and total cost of $30.58/kg dried product^?1     

Optimization of Crotonaldehyde Oxidation Catalyst using Response Surface Methodology

Crotonic acid was produced by oxidation of crotonaldehyde over molybdophosphoric acid supported on activated carbon. The full 2³ central composite design was performed and aimed at optimizing oxidation catalysts to maximize the yield of crotonic acid. Response surface methodology was applied to obtain a second‐order polynomial model and to generate the optimum conditions, with a loading of molybdophosphoric acid of 0.25, mass ratio of catalyst to crotonaldehyde of 0.025 and mass ratio of vanadium pentoxide to molybdophosphoric acid of 0.08. The crotonic acid yield was 66.7 % under these conditions. Three experiments were conducted using the same optimum conditions, and therefore, good agreement was observed between the experimental data and the predicted values obtained from the model, by comparison     

Optimization of Food Waste Bioevaporation Process Using Response Surface Methodology

A proven bioevaporation process was used to treat food waste (FW) by mixing ground FW with biodried sludge (BS). Organic loading (OL), moisture content (MC), and air flow rate (Q_g) showed significant influences on FW bioevaporation performance. Single-parameter experiments for MC and Q_g were conducted and ranges were determined to be 55–67 wt% and 0.04–0.14 m³/kg TS_mixture · h, respectively. In order to optimize the FW bioevaporation process, a central composite design (CCD) and response surface method (RSM) were applied over the preselected ranges of OL (0.00–0.16 kg VS_FW/kg TS_BS), MC (50.91–71.09 wt%), and Q_g (0.01–0.17 m³/kg TS_mixture · h). The results indicated that OL of 0.06 kg VS_FW/kg TS_BS, MC of 59.2 wt%, and Q_g of 0.09 m³/kg TS_mixture · h were the optimal conditions for the FW bioevaporation process. Water evaporation of 123.1% and VS degradation of 108.4% were obtained under these estimated optimal conditions.     

Optimization of Ultrasonic Enhanced Salt‐Containing Hydrodistillation by Response Surface Methodology

An ultrasonic enhanced salt‐containing hydrodistillation (UESHD) method for separating essential oil from lavender (Lavandula angustifolia) flowers was investigated using response surface methodology (RSM). The experimental data obtained from a 27‐run experiment were fitted to a second‐order polynomial equation. The optimal conditions were determined by the 3D response surface and the contour plots derived from the models. The efficiency of UESHD and conventional hydrodistillation (HD) was compared. The extraction yield of UESHD was two‐fold higher than that of HD. In addition, GC‐MS results indicated some differences in composition and content between the two essential oils from UESHD and HD.     

Optimization of Phospholipid Nanoparticle Formulations Using Response Surface Methodology

The present study deals with the optimization of phospholipid liposome formulations to mimic red blood cells. Optimization of different concentrations of distearylphosphatidylcholine, dipalmitoylphosphatidylcholine, and phosphatidylserine at a fixed concentration of lecithin and Tween^® 80 was done using response surface methodology. The optimized formulation produced liposomes with a particle size in the range of 112–196 nm. The optimized formulation shows low encapsulation efficiency at low levels of insulin but increases at higher loading levels. Formulated vesicles fulfill the size requirement for intravenous drug delivery. The present system is environmentally friendly with respect to biodegradability and biocompatibility.     

Optimization of Enzymatic Synthesis of Tricaprylin in Ionic Liquids by Response Surface Methodology

Ten 1,3‐dialkylimidazolium‐based ionic liquids (ILs) have been investigated as media for the enzymatic synthesis of tricaprylin, in comparison with the conventional organic solvent hexane. The results suggested that the esterification activity of Novozym 435 was higher than Lypozyme RM IM in all the ILs assayed. Novozym 435 showed higher catalytic activity in ILs with anions Tf₂N^? and PF₆^? than in BF₄^? and hexane. FTIR analysis of the secondary structure of the lipase indicated that a smaller decrease of the α‐helix was observed in [C₄MIM] Tf₂N and [C₄MIM] PF₆ than [C₄MIM] BF₄ and hexane, indicating that the anions of ILs might be a key factor for the activity of lipase in ILs. Process parameters (amount of lipase, caprylic acid/glycerol molar ratio, temperature and their interactive effects) were optimized in 1‐butyl‐3‐methylimidazolium hexafluorophosphate ([C₄MIM]PF₆) using Novozym 435 by response surface methodology. When the reactions were performed with the lipase amount of 6.1 % substrate mass at a caprylic acid/glycerol molar ratio of 4.5:1 and 66.7 °C, a higher yield was reached up to 92.4 %.     

Optimization of Microwave-Vacuum Drying Parameters of Saskatoon Berries Using Response Surface Methodology

A combined microwave and vacuum system was used to dry the Saskatoon berries (Amelanchier alnifolia). A central composite rotate design and response surface methodology were used to determine the influence of process variables (microwave power, drying time, and fruit load) and arrive at optimal processing conditions to reduce the moisture content and water activity of the berries to a safe level. It is concluded that the yield of moisture content and water activity can be reduced to 20% and 0.50, respectively, for microwave power 5.7–6 kW, drying time 51.5–55 min, and fruit load 10–9.75 kg.     

Supercritical CO2 Extraction Optimization of Onion Oil Using Response Surface Methodology

Response surface methodology was employed to optimize the conditions of supercritical CO₂ extraction of the oil from freeze‐dried onion powder. The effects of pressure, temperature and extraction time on the yield of oil were investigated. The maximum extraction yield of 4.69 ± 0.04 g/kg dry basis was achieved at a pressure of 20.6 MPa, a temperature of 40.6 °C, a time of 260 min, a CO₂ flow rate of 22 L h^–1, and an entrainer ratio of 0.1 mL absolute ethanol per gram dry basis. The chemical composition of the oil was analyzed by gas chromatography‐mass spectrometry. The most representative compounds of the essential oil were organosulfur‐containing compounds and, among these, the main constituents were methyl 5‐methylfuryl sulfide (18.30 %), methyl 3,4‐dimethyl‐2‐thienyl disulfide (11.75 %) and 1‐propenyl propyl disulfide (9.72 %).     

响应面优化法研究蔗糖-对苯二酚树脂胶粘剂合成

以蔗糖,对苯二酚为原料,根据中心复合实验设计原则,在单因素实验的基础上采用响应面优化法,建立了粘度与各影响因子的回归方程,并得到以粘度为响应值的响应面图,进而得出蔗糖-对苯二酚树脂胶粘剂合成的最佳工艺条件:反应温度89.3℃,反应时间5.9 h,原料比为1.79,催化荆用量10%,在此条件下,测得的粘度为8.4×500...     

Amoxicillin Extraction from Aqueous Solution by Emulsion Liquid Membranes Using Response Surface Methodology

The extraction of amoxicillin (AMX) from aqueous solutions by emulsion liquid membranes (ELMs) was investigated for the first time. The liquid membrane phase of the ELM consisted of Aliquat 336 as carrier, Span 80 as surfactant, n‐hexane as diluent, and sodium chloride solution as internal phase. Response surface methodology (RSM) based on central composite design (CCD) was applied to evaluate and optimize the effects of several parameters such as carrier concentration, feed concentration, internal phase concentration, and treat ratio (volume ratio of the external phase to the emulsion phase). A polynomial model was fitted to predict the extraction yield of AMX. Under optimized conditions, the highest extraction yield of AMX was 99.8 %.     

Optimization of Lipase-Catalyzed Interesterification of Flaxseed Oil and Tricaprylin Using Response Surface Methodology

The biosynthesis of structured lipids (SL) in organic solvent media was carried out by the interesterification of flaxseed oil (FO) and tricaprylin (TC), using Novozym 435. The bioconversion yield (BY, %) of medium-long-medium type SL, including C-caprylic and Ln-linolenic acids (CLnC), La-linoleic acid (CLaC) and O-oleic acid (COC), was monitored. Response surface methodology was used to obtain significant models for the responses, on the basis of a five level, five variable central composite rotatable design. In the experimental preliminary trials significant reaction parameters, including reaction temperature (T _r), TC/FO molar ratio (M _r), enzyme concentration (E _c), reaction time (R _t) and initial water activity (a _w), were considered for optimization. Significant models for CLnC, CLaC and COC were determined after regression analysis with backward elimination. The optimal conditions, generated for a maximum CLnC, CLaC and COC, were found to be 54.50–56.25 °C for T _r, 6.23–6.25 mol/mol for M _r, 2.68–3.13 % for E _c, 36.58–37.50 h for R _t and 0.15–0.33 for a _w. Under these optimum conditions, the BY of CLnC, CLaC and COC was predicted to be 32.48–36.67, 3.26–3.38 and 5.79–6.16 %, respectively.     

Chemical Characterization and Physical Properties of Solvents Derived from Epoxidized Methyl Soyate

Reactions of epoxidized methyl soyate (EMS) with alcohols, carbon dioxide, and acetone yielded liquids with solvent properties that make them more suitable than methyl soyate for dissolving polar substances. The reactions of EMS in the presence of Amberlyst‐15 with alcohols, including methanol, ethanol, n‐butanol, and 2‐methoxyethanol, produced a series of solvents containing ether (–OR) and alcohol (–OH) groups. Reactions of EMS with carbon dioxide and acetone gave products with carbonate and ketonide functional groups, respectively. The complex mixture of compounds present in the product, EMS(MeOH), resulting from the reaction of EMS with MeOH, was characterized by MS and NMR investigations. In addition to products resulting from MeOH addition across the epoxide ring, were major amounts of cyclic tetrahydrofuran derivatives that were derived from reactions of methyl linoleate (18:2) with MeOH. All of the solvents were characterized by high boiling points and low vapor pressures. Their viscosities were higher than that of methyl soyate. Especially notable were their very high Kauri‐butanol values, which ranged from 280 to 852, all of which are much higher than that (57) of methyl soyate. Such high KB values indicate that these solvents have very favorable solubilizing properties, which is illustrated by the ability of EMS(MeOH) to readily dissolve both polar (e.g., MeOH) and non‐polar (e.g., hexane) compounds.     

Optimization of Fluidized Bed Drying Process of Green Peas Using Response Surface Methodology

The fluidized bed drying process of green peas was optimized using the response surface methodology for the process variables: drying air temperature (60–100°C), tempering time (0–60 min), pretreatment, and mass per unit area (6.3–9.5 g/cm²). The green peas were pretreated by pricking, hot water blanching, or chemical blanching. Product quality parameters such as rehydration ratio, color, texture, and appearance were determined and analyzed. Second-order polynomial equations, containing all the process variables, were used to model the measured process and product qualities. Rehydration ratio was influenced mostly by pretreatment followed by tempering time, temperature, and mass per unit area. Pretreatment and mass per unit area significantly affected color and texture. Higher levels of temperature and lower levels of tempering time and mass per unit area increased the rehydration ratio. The optimum process conditions were derived by using the contour plots on the rehydration ratio and sensory scores generated by the second-order polynomials. Optimum conditions of 79.4°C drying air temperature, 35.8-min tempering time, pretreatment of the once pricked peas with chemical blanching in a solution of 2.5% NaCl and 0.1% NaHCO₃, and mass per unit area of 6.8 g/cm² were recommended for the fluidized bed drying of green peas. At these conditions the rehydration ratio was 3.49.     

Mercury Removal by Adsorption on Pectin Extracted from Sugar Beet Pulp: Optimization by Response Surface Methodology

Considering the rich sugar beet resource in Xinjiang, China, the possibilities for Hg(II) removal by pectin extracted from sugar beet pulp and optimization of the extraction process using response surface methodology (RSM) were studied. The experiments were proposed by Box‐Behnken design (BBD) and a second‐order regression model was developed for regression analysis and analysis of variance. Optimized conditions in terms of temperature, concentration, and solid‐liquid ratio were determined. The effects of different parameters like pH, time, temperature, and initial Hg(II) concentration on adsorption capacity were investigated. The isotherm adsorption experiments were fitted with the Langmuir model which indicated monolayer adsorption.     

响应面法优化季戊四醇三烯丙基醚合成

以季戊四醇、氢氧化钠和氯丙烯为原料,在相转移催化剂作用下,经Williamson醚化反应合成季戊四醇三烯丙基醚。采用响应面法探讨了反应温度、NaOH的质量分数和催化剂四丁基溴化铵用量等因素对产品收率的影响,并建立了相应的预测模型。结果表明:NaOH的质量分数和催化剂四丁基溴化铵用量这两个因素对收率影响显著,温度和催化剂四丁基溴化铵的用量交互效应影响显著。得到了季戊四醇三烯丙基醚合成的最适宜工艺条件:四丁基溴化铵作催化剂,反应温度为78.0℃、NaOH的质量分数为54.9%、催化剂与三羟甲基丙烷的质量之比为11.1%时获得最高收率70.2%。     

响应面法优化达托霉素发酵培养基的研究

通过Plackett-Burman设计、最陡爬坡设计与响应面设计,对达托霉素发酵培养基进行了优化,并使用Design expert 7.0软件对实验结果进行分析.结果表明,培养基各成分中影响达托霉素产量的主要因素是糊精、可溶性淀粉和L-天冬氨酸,其最佳浓度分别为7.0g·L-1、6.66 g·L-1、0.4g·L-1,在此条件下,达托霉素的产量达到185.3 mg· L-1,较优化前提高了73.7％.