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First, a chlorinator was self-designed in this paper, and dichloride of 2-methyl-1-propene was synthesized by 2-methyl-1-propene reacted with chlorine fast in this reactor. By means of the Orthogonal Experiments design and single factor experiments, the influence of several reaction variables on the yield were examined and the optimum reaction conditions under the intervallic operation were obtained, the yield and selectivity of dichloride of 2-methyl-1-prop-ene were more than 65% and 80% respectively. Second, the preparation of 2-methylene-1, 3-propanediol, which dichloride of 2-methyl-1-propene reacted with alkali was investigated. By means of the Orthogonal Experiments design and single factor experiments, the influence of several reaction variables on the yield were examined and the optimum reaction conditions under the intervallic operation were obtained, the conversion of dichloride of 2-methyl-1-propene was 100%. Moreover the preparation of MPO, which 2-methylene-1, 3-propanediol reacted with hydrogen, in presence of Al_2O_3-Pd catalyst, was gotten, and the product was appraised.

本文在氯化反应过程中,自行设计制作出了氯化管式反应器,在该反应器中异丁烯和氯气迅速混合反应生成二氯异丁烯,根据该氯化反应特征利用正交试验和单因素试验考察了有关因素的影响并优化得到了最佳工艺条件,二氯异丁烯的总收率达65%以上,选择性达80%;接着,对二氯异丁烯进行水解反应制得了2-甲烯-1,3-丙二醇,讨论了相关因素对水解反应的影响,并通过正交试验和单因素试验得到了较佳工艺条件,二氯异丁烯的转化率达100%;同时还对制备的2-甲烯-1,3-丙二醇在常压下采用三氧化二铝负载钯催化剂催化加氢得目的产物MPO,并对产品进行了鉴定,从而打通了整个工艺路线。

Reaction temperature, reaction time and different distillate oil on the properties of petroleum sulfonate were studied.

本文以发烟硫酸和三氧化硫作为磺化剂,选用重烷基苯或石油馏分油,在不同的工艺条件下进行磺化反应,摸索了反应物配比、反应温度、反应时间和不同原料等条件对合成产物的性能影响,得出反应物配比是影响磺化收率的重要因素。

The reaction time, reaction temperature and catalyst influencing on esterification were investigated, and the acid value, flashing point and other properties were determined.

考察了反应时间、反应温度、催化剂等反应条件对酯化反应的影响,并对增塑剂的酸值、闪点及其他主要性能指标进行了测定,改进了酯化反应工艺条件,讨论了样品色泽、酸值及闪点的影响因素。

Two representative compounds have been determined by X-ray crystallography. The best ratio of reactants, the adequate reaction temperature and solvent have been found by contrast experiments.4. The better photoreaction conditions and irridation times have been confirmed through the different photoreaction results. It is the first time that fifty quinazoline derivatives with biological activity and four photooxidation products with urea functional groups have been obtained by photochemistry method. Two representative compounds, quinazoline derivatives and photooxidation products, have been determined by X-ray crystallography, respectively.

通过实验对比我们找到了较佳的反应物的投料比、反应温度和反应所用的溶剂。4、根据不同条件下的光反应结果,确定了硫脲衍生物的相对较好的光反应条件和光照时间,首次利用光化学手段成功得到50个具有生物活性的喹唑啉衍生物和4个具有脲基官能团的光氧化的产物,测定了两个具有代表性的喹唑啉和光氧化的产物的晶体结构。

It was increased ethyl hexanoate synthesis substrate concentration mediated by Rhizopus chinensis 2113 whole-cell lipase after improved synthetic activity and optimized reaction condition. The reaction condition were: caproic acid concentration 2.4mol/L, substrate molar concentration ratio 1:1.1, initial water content ≤0.2%, lipase water activity 0.3~0.66, enzyme amount 16%, reaction temperature 30℃, agitation speed 150 r/min.

通过合成酶活的提高及反应条件的优化,提高了华根霉2113全细胞脂肪酶催化己酸乙酯合成的反应底物浓度,其反应条件为:己酸浓度为2.4mol/L;酸醇摩尔浓度比1:1.1;反应体系含水量≤0.2%;脂肪酶水活度0.3~0.66;加酶量16%;反应温度30℃;150r/min振荡反应。

The influences of polymerization conditions such as the dosage of cyanobenzene, catalyst, co-catalyst and polymerization temperature on the polymerization (gelation time and monomer conversion) and the swelling value of PDCPD were investigated.

考察了主要反应条件如苯甲腈的用量、聚合反应温度、主催化剂的用量和助催化剂的用量等对聚合反应速率、聚合反应转化率和PDCPD膨胀值的影响,并得到了最优的聚合反应条件:苯甲腈与WCl_6的摩尔比为3,聚合反应温度为70℃,DCPD与WCl_6的摩尔比为1500,Et_2AlCl与WCl_6的摩尔比为11。

Solid superacids SO~2-_4/TiO_2-Al_2O_3 were prepared and used to catalyze the esterfication of iso-octyl alcohol and by-products in oxidization reaction of durene,which were pretreated before esterifying reaction.

考察了催化剂用量、异辛醇与混合酸的质量比、反应时间等因素对酯化反应的影响,确定了较佳的反应工艺条件:m∶m∶m=0.01∶3.18∶1,反应时间为3 h,在此反应条件下预处理后的混合酸转化率可达到99.9%。

The results show that the optimal parameters of esterification are as follows: 4% of SO42-/ZrO2, molar ratio of methanol to litsea cubeba kernel oil 101, 68 ℃ of reaction temperature and 4 h of reaction time, the acid value decreases to 2.52 mg/g. Compared with the traditional acidic-catalyzed method, this method has the advantages of no acid proof equipment, easy to recycle catalyst and no acidic waste water emission. The optimal parameters of transesterification are as follows: 25 ℃ of reaction temperature, 0.5% of hexadecyl-trimethyl-ammonium bromide, 1% of NaOH, molar ratio of methanol to the oil 61 and 15 min of reaction time. The ester exchanging rate is 97.6%. This method adopts phase transfer catalyst and produces industry prospect, which has many advantages such as energy-saving and time-saving under room temperature.

研究结果表明,固体酸SO42-/ZrO2催化酯化反应的最佳条件为:油重4%的SO42-/ZrO2,醇油摩尔比为101,温度为68 ℃,反应时间为4 h,原油酸值降到2.52 mg/g;该法相对浓硫酸催化酯化法具有不需耐酸设备、催化剂易回收、无废水排放等优点;相转移催化酯交换反应的最佳条件为:温度为 25 ℃,0.5%的十六烷基三甲基溴化铵,油重1%的NaOH,醇油摩尔比为61,反应15 min,原油酯交换率达到97.6%;采用相转移催化技术,反应在常温下进行,大大减少了能耗,缩短了反应时间,具有的产业化前景。

The reaction has been drawing increased attention in that the reaction permit the use of organoboron compounds that are thermally stable and inert to water and oxygen.In this section microwave promoted Suzuki reaction of Sodium tetraphenylborate (NaBPh4) with carboxylic anhydrides catalyzed by Pd(PPh3)2Cl2 in THF was first reported.

第二章:微波辐射下Pd配合物催化NaBPh_4与羧酸酐的偶联反应研究本章中我们在微波辐射条件下,研究了PdCl_2(PPh_3)_2催化NaBPh_4与羧酸酐偶联反应,合成出了十种不对称芳酮,并分别考察了微波辐射功率、辐射时间、溶剂和原料配比等因素对反应的影响,优选出了较佳的反应条件,并根据文献及实验结果,讨论了可能的反应机理。

The Suzuki reaction, the coupling of organoborate compounds with organic electrophiles catalyzed by Palladium complexes, is a valuable Csp2-Csp bond forming reaction. The reaction has been drawing increased attention in that the reaction permit the use of organoboron compounds that are thermally stable and inert to water and oxygen.In this section microwave promoted Suzuki reaction of phenylboronic acid with benzyl halides catalyzed by Pd(PPh3)2Cl2 DMF/H2O(v/v=10 : 2) was first reported.

第四章:微波辐射下Pd配合物催化端烯与芳卤偶联反应研究本章中我们在微波辐射条件下,研究了PdclZ(P Ph3):催化端烯与芳卤的偶联反应,合成出了七种乙烯基化合物;并分别考察了微波辐射功率、辐射时间、原料配比、和PTc等因素对反应的影响,优选出了较佳的反应条件,并根据文献及实验结果,讨论了可能的反应机理。

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