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In the one half part, according to the strontium nature, thermodynamic calculation of correlative reaction and the principle of the vacuum aluminothermy reduction process, with the laboratory findings of preparation strontium by vacuum aluminothermy reduction compared and analyzed in different parameter conditions, a variety of factors which effect the decomposition rate of SrCO_3 and the percent reduction of strontia are gotten out. The factors include that the decomposition rate of SrCO_3 is influenced by different addition and pressure. They also include that the percent reduction of strontia is influenced by excess coefficient of reducing agent aluminium powder, the particle size of raw material or reducing agent, the pressure of barbecuing, temperature and reduction time. According to those, we can draw the conclusion as follows:(1) Decomposition temperature of SrCO_3 is decreased by adding carbon and alumina in different degree.(2) With quantitative carbon added under the vacuum condition, the decomposition temperature of SrCO_3 is decreased obviously, which can fall 150℃ compared with atmospheric pressure.(3) In keeping 1150℃ of 2.5h, under the 5Pa vacuum condition, the decomposition rate of SrCO_3 nearly keeps in 99% steadily.

在前半部分的真空铝热还原法中,根据锶的性质、相关反应的热力学计算及真空铝热还原法原理,通过对不同参数条件下的真空铝热还原法生产金属锶的实验结果的分析比较,得出了影响SrCO_3的分解率和氧化锶的还原率的种种因素,具体因素包括不同添加剂、不同气压对SrCO_3分解率的影响,还原剂铝粉的过量系数、原料与还原剂的粒度、制团压力、温度和还原时间等对氧化锶还原率的影响,得出具体结论如下:(1)添加碳和Al_2O_3能不同程度的降低SrCO_3的分解温度;(2)真空条件下加入一定量的碳可显著降低SrCO_3的分解温度,比之常压下可降低150℃之多;(3)在1150℃恒温2.5h、真空度达到5Pa的条件下,SrCO_3的分解率几乎保持稳定在99%;(4)氧化锶的还原率随还原剂过量系数的增大而增大,但是趋势越来越小,当过量系数超过25%后,氧化锶的还原率几乎不再增加;(5)氧化锶的还原率随原料与还原剂的粒度的变细而增加;(6)氧化锶的还原率随制团压力的增加而增加,但超过一定值后,氧化锶的还原率反而会下降;(7)氧化锶的还原率随还原温度的升高而增加;(8)氧化锶的还原率随还原时间延长而增加,在本实验条件下,超过2.5h趋于稳定。

Ionone was synthesized from Litsea cubeba oil and lemen oil ,and condition of condensation,cyclization and purification of product was studied.

以山苍子油、柠檬草油为原料合成紫罗兰酮,研究了缩合反应、环化反应、产品精制的工艺条件;并缩合反应中,柠檬醛的转化率为99%以上,产品得率95%;环化反应中,假性紫罗兰酮的转化率98%以上,产品得率90%。

In chapter 4 an abnormal reaction that the nitro group of 1-aryl-2-nitroethenescan be easily replaced by the organic moity of FG-RZnI using Ni〓 and tertiaryamine as catalyst was first given. The experimental results show that in the presenceof catalytic amount of Ni〓 and tertiary amines, the reaction of FG-RZnI andl-aryl-2-nitroethenes give the substitution products l-aryl-l-alkene, instead ofMichael addition products.

通过实验发现,在催化量的Ni〓及叔胺催化下, l-硝基-2-芳基乙烯与烷基碘化锌并不进行Michael加成反应,而是发生1-硝基-2-芳基乙烯中硝基被取代的反应,生成了高产率的1-芳基-l-烯烃,由于此反应的原料易得、反应条件温和、产物的产率高,因而是合成l-芳基-1-烯烃的有效方法。

A compound 2-(3-hydroxyphenyl)[60] fullerene pyrrolidine was synthesized by the 1,3-dipolar cycloaddition reaction of the fullerene(C60) and azomethine ylide (prepared from glycine and 3-hydroxybenzaldehyde). The product was characterized by UV-Vis,1H-NMR ,FT-IR and MS. The reaction conditions affecting the yields of product were investigated and the optimum reaction conditions with product yield 75%(based on consumed C60) were:molar ratio of C60∶3-hydroxybenzaldehyde:glycine 1∶3∶6,reaction temperature 95℃,reaction time 18h.

利用甘氨酸和3-羟基苯甲醛与C60发生1, 3-偶极环加成反应,合成分离得到了2-(3-羟基苯基)[60]富勒烯吡咯烷,用UV-Vis、1H-NMR、FT-IR、MS等测试手段表征了产物的结构,并通过单因素方法,探讨了反应条件对产物产率的影响,得到最佳工艺条件:反应物摩尔比1∶3∶6,温度95 ℃,反应时间18 h,产物的产率可达75%(以消耗的C60计)。

To be different from the already chloromethylation catalyst, it has a certain amount of moisture wet, which will not produce huge amounts of doughtic cancerogenic chloromethyl methyl ether during and after the reaction.4,4\'-bisbiphenyl, 1,4-bisbenzene, 1,4-bis(chloro- methyl)-2,5-dimethylbenzene, 1,5-bis-2,4-dimethylbenzene, 4-(chlor- omethyl)-1,2-dimethylbenzene, 1,2-bis-4,5-dimethylbenzene, 5,8-bis-1,2,3,4-tetrahydronaphthalene, 3,3\',5-tris-4,4\'-bisbiphenyl and 3,3\', 5,5\'-tetrakis-4,4\'-bisbiphenyl were synth- esized by using this new catalyst. Results indicated that when the reaction temperature was 55~60℃, the reaction time was 12h, the catalyst which consists of the concentration of 80%H_2SO_4, HAc and Lewis acid, the amount of Lewis acid 0.15 mol(nLewis:nbiphenyl=1.5:1), yield of biphenyl chloromethylation product 4,4\'-bis(chrolomethylbiphenyl can reach a maximum 85%.

采用这种催化体系完成了4,4′-二氯甲基联苯、对二氯甲基苯、1,4-二氯甲基-2,5-二甲基苯、1,5-二氯甲基-2,4-二甲基苯、4-氯甲基-1,2-二甲基苯、1,2-二氯甲基-4,5-二甲基苯、5,8-二氯甲基-四氢萘、3,3',5-三氯甲基-4,4'-二甲基苯和3,3',5,5'-四氯甲基-4,4'-二甲基苯的合成,结果表明:在反应条件为:反应温度55~60℃,反应时间12h,选择80%H_2SO_4、冰醋酸和Lewis酸为催化剂,反应最佳反应Lewis酸用量是0.15mol(和原料比为1.5:1),反应效果最好,联苯氯甲基化产物(4,4′-二氯甲基联苯)收率为85%;在反应条件为:反应温度70℃,反应时间8h,80%H_2SO_4、冰醋酸和Lewis酸为催化剂,反应最佳反应Lewis酸用量是0.1mol(和原料比为1:1)时,反应效果最好,苯的氯甲基化产物收(来源:ABd0C论文eded网www.abclunwen.com)率为75%;在反应条件为:在反应条件为:反应温度40℃,反应时间10h,60%H_2SO_4和Lewis酸为催化剂,反应最佳反应Lewis酸用量是0.1mol(和原料比为1:1)时,反应效果最好,对二甲苯氯甲基化产物(1,4-二氯甲基-2,5-二甲基苯)收率为78.5%;在反应条件为:反应温度35℃,反应时间10h,60%H_2SO_4、冰醋酸和Lewis酸为催化剂,反应最佳反应Lewis酸用量是0.1mol(和原料比为1:1)时,反应效果最好,间二甲苯氯甲基化产物(1,5-二氯甲基-2,4-二甲基苯)收率为81.5%。

Its mechanism is the use of anthraquinone in alkali conditions off proton surface forming 10 more stable carbon anion face, but because carbon anion and oxygen ion exist between testosterone and enolate type each other changes, cause reaction product complex, at least five, reaction selectivity, product yield, separation difficulties, and product purity is not high, therefore, using the type and quantity of alkali, phase transfer catalyst type, solvent, to optimize the selection process conditions so as to improve the yield target product.

其机理是利用蒽酮在碱存在的条件下脱去氢质子面形成10位较稳定的碳负离子面进行,但是因为碳负离子和氧负离子之间存在酮式和烯醇式的互变,导致反应复杂,产物至少有五种,反应选择性差,产物分离困难,产率低,且产品纯度不高,因此,利用对碱的种类和量的多少,相转移催化剂的种类,反应溶剂的选择,来优化反应工艺条件从而提高目标产物的产率。

To improve the yield of an Amide-type Tripodal Ligand and investigate its coordination with rare earth ion under mild condition,a series of Amide-type Tripodal Ligands(L1—L4) have been prepared by the reactions of nitrilotriacetic acid and oxalyl chloride with four kinds of amides,respectively.

为了提高酰胺型三脚架型配体的产率,进一步研究其与稀土离子的配位形式及配合物的荧光性能,以氨三乙酸为母体,草酰氯为氯化试剂,与4种胺在较温和的条件下合成了具有三脚架型结构的配体(L1—L4),并考察了实验条件、反应温度、反应体系溶剂、缚酸剂、反应时间及催化剂对反应产率的影响。

Kinetic spectrophotometric method for the determinationof trace nitrilotriacetic acid;2. To improve the yield of an Amide-type Tripodal Ligand and investigate its coordination with rare earth ion under mild condition,a series of Amide-type Tripodal Ligands(L1—L4) have been prepared by the reactions of nitrilotriacetic acid and oxalyl chloride with four kinds of amides,respectively.

为了提高酰胺型三脚架型配体的产率,进一步研究其与稀土离子的配位形式及配合物的荧光性能,以氨三乙酸为母体,草酰氯为氯化试剂,与4种胺在较温和的条件下合成了具有三脚架型结构的配体(L1—L4),并考察了实验条件、反应温度、反应体系溶剂、缚酸剂、反应时间及催化剂对反应产率的影响。

Third, we studied the N-alkylation of phthalimide, indole, benzimidazole, succinimide with a variety of halogen in ionic liquid [BF4], [PF_6]. The present method has many obvious advantages, compared to those reported in the literature, including the generality, simplicity of the methodology, the ease of product isolation, the higher yield and potential for recycling of ionic liquids.

第三、研究了离子液体[BF_4]、[PF_6]和BF_4促进邻苯二甲酰亚胺、吲哚、苯并咪唑、丁二酰亚胺的N-烷基化反应,克服了传统溶剂中进行N-烷基化反应要求强碱、反应条件苛刻、时间长、产率一般的不足,改善了反应条件、提高了产率。

A new fullerene derivative containing energy-producing groups was prepared, and the reaction conditions affecting the yield were studied by the kroenecker method. The optimal reaction conditions with a 53.5% yield (based on consumed C60) are: 1:3:6 of molar ratio of C60 , o–nitrobenzaldehyde and sarcosine , 55℃ of reaction temperature, 12 h of reaction time, 40mL of toluene solvent.

利用N-甲基甘氨酸、邻-硝基苯甲醛和C60反应,合成分离出了含有硝基的新型富勒烯吡咯烷衍生物,通过正交试验对其工艺条件进行了研究,探讨了反应物剂量比、温度、时间和溶剂体积对产物产率的影响,得到了合成产物的最佳工艺条件:反应物剂量比为1:3:6、温度为55℃、反应时间为12h、溶剂甲苯体积为40mL,此时产物产率可达到53.5%(以消耗的C60计)。

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