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为了降低溴硝醇生产的溴素消耗,采用甲醛和硝基甲烷经过缩合、中和、溴化和氯化过程合成了溴硝醇。优化反应条件为缩合反应温度0~4℃,反应时间60 min;中和反应温度0~4℃,反应时间67 min;溴化反应温度-4℃以下,反应时间90 min,溴素过量5%。新工艺溴硝醇收率79.1%,含量99.7%,最大杂质含量0.09%。与传统工艺相比溴素平均消耗降低48%,原料成本降低约27.2%。 相似文献
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通过对硝基甲烷先进行溴代反应生成溴代硝基甲烷,再与甲醛进行加成反应的新方法合成布罗波尔,不仅避免了使用有毒易燃非极性有机溶剂,而且使产品的总收率达到912%。 相似文献
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Bronopol (2‐bromo‐2‐nitropropane‐1,3‐diol) is used as preservative in cosmetic industry. Its main role in commercial products consists in protection of the cosmetic composition stability by inhibiting the development of micro‐organisms. Unfortunately, preservatives can also undergo the degradation processes. The aim of examinations was to prove that bronopol decomposes in aqueous solutions and storage conditions have a significance influence on its degradation rate. High‐performance liquid chromatography method (methanol/water with hydrochloric acid 5:95 v/v) with spectrophotometric detection (210 nm) was used for examining the decomposition rate of bronopol. The impact of chemical (addition of cosmetics components: citric acid and/or sodium dodecylsulfate) and physical (elevated and ambient temperature, sunlight or ultraviolet radiation and air access) factors has been elaborated. Bronopol decomposes most rapidly (independently on the sample surrounding conditions) when it is in solution with sodium dodecylsulfate, the inverse dependence is observed in the presence of two compounds – citric acid and sodium dodecylsulfate. Additionally, the elevated temperature causes the acceleration of decomposition. Bronopol degradation by‐products were also identified as methanol, formic acid, tris(hydroxymethyl)methane and 2‐bromo‐2‐nitroethanol. 相似文献
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Milk urea N (MUN) is used by dairy nutritionists and producers to monitor dietary protein intake and is indicative of N utilization in lactating dairy cows. Two experiments were conducted to explore discrepancies in MUN results provided by 3 milk processing laboratories using different methods. An additional experiment was conducted to evaluate the effect of 2-bromo-2-nitropropane-1, 3-diol (bronopol) on MUN analysis. In experiment 1, 10 replicates of bulk tank milk samples, collected from the Pennsylvania State University's Dairy Center over 5 consecutive days, were sent to 3 milk processing laboratories in Pennsylvania. Average MUN differed between laboratory A (14.9 ± 0.40 mg/dL; analyzed on MilkoScan 4000; Foss, Hillerød, Denmark), laboratory B (6.5 ± 0.17 mg/dL; MilkoScan FT + 6000), and laboratory C (7.4 ± 0.36 mg/dL; MilkoScan 6000). In experiment 2, milk samples were spiked with urea at 0 (7.3 to 15.0 mg/dL, depending on the laboratory analyzing the samples), 17.2, 34.2, and 51.5 mg/dL of milk. Two 35-mL samples from each urea level were sent to the 3 laboratories used in experiment 1. Average analyzed MUN was greater than predicted (calculated for each laboratory based on the control; 0 mg of added urea): for laboratory A (23.2 vs. 21.0 mg/dL), laboratory B (18.0 vs. 13.3 mg/dL), and laboratory C (20.6 vs. 15.2 mg/dL). In experiment 3, replicated milk samples were preserved with 0 to 1.35 mg of bronopol/mL of milk and submitted to one milk processing laboratory that analyzed MUN using 2 different methods. Milk samples with increasing amounts of bronopol ranged in MUN concentration from 7.7 to 11.9 mg/dL and from 9.0 to 9.3 mg/dL when analyzed on MilkoScan 4000 or CL 10 (EuroChem, Moscow, Russia), respectively. In conclusion, measured MUN concentrations varied due to analytical procedure used by milk processing laboratories and were affected by the amount of bronopol used to preserve milk sample, when milk was analyzed using a mid-infrared analyzer. Thus, it is important to maintain consistency in milk sample preservation and analysis to ensure precision of MUN results. 相似文献
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采用先羟甲基化后溴化反应的方法合成布罗波尔,通过正交试验考察了原料配比、反应时间、反应温度对反应结果的影响,得到的较佳反应条件如下:n(硝基甲烷):n(氢氧化钠):n(甲醛):n(溴素)=1:1:2:1,羟甲基化反应温度20℃,反应时间1.5h,溴化反应温度15℃。考察了布罗波尔在单一及复配溶剂中的溶解度和重结晶试验,确定的较佳复配溶剂比m(乙酸乙酯):m(氯仿)=1:1。在较佳反应条件下,反应过程收率可达90%,重结晶单程收率可达83%,得到的产品纯度在99%以上。 相似文献
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Our objective was to determine the effect of commonly used milk preservatives on the accuracy of fat, protein, and lactose content determination in milk by mid-infrared (mid-IR) milk analysis. Two producer raw milks (Holstein and Jersey) and 2 pasteurized modified milks, 1 similar to Holstein milk and 1 similar to Jersey milk were used as the 4 different milk sources. Seven different milk preservative approaches (K2Cr2O7 and 6 different bronopol-based preservatives) and a portion of unpreserved milk for each of the 4 different milks sources were tested for fat B, lactose, protein, and fat A. The experiment was replicated 3 times (28 d each) for a total of 84 d. Two mid-infrared (mid-IR) transmittance milk analyzers (an optical and a virtual filter instrument) were used. A large batch of pilot milk was prepared from pasteurized, homogenized, unpreserved whole milk, split into vials, quick frozen by immersion in liquid nitrogen, and transferred into a −80°C freezer. Pilots were thawed and analyzed on each testing day during the study. Significant increases were observed in all uncorrected readings on the pilot milks over the 84 d of the study, but the increases were gradual and small on each instrument for all components. Results from the study were corrected for these changes. A significant difference in mid-IR fat A readings was observed, whereas no differences were detected for fat B, lactose, or protein between unpreserved and preserved milks containing 0.02% K2Cr2O7. Therefore, K2Cr2O7 has little or no effect on mid-IR test results. All bronopol-based preservative approaches in this study differed in mid-IR test results compared with K2Cr2O7-preserved and unpreserved milks, with the largest effect on protein results. Mid-IR uncorrected readings increased with time of refrigerated storage at 4°C for all preservative approaches, with the largest increase for protein. The rate of increase in uncorrected readings with time of storage was always higher for raw milks than for pasteurized milks, and the stability of instrument zero was lower for raw milks than for pasteurized milks. The largest economic effect of a systematic bias caused by a preservative occurs when the milks used for calibration and routine testing for payment do not contain the same preservative or when calibration milks are preserved and milks for routine testing are unpreserved. These effects can create errors in payment for large dairy processing plants ranging from several hundred thousand to over a million dollars annually. 相似文献
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