Liquid-liquid extraction technology in the application of pesticide intermediates synthesis of phenol
phenol in many natural products in the form of monomers or polymers was found. It has extensive application in pesticide, such as adjacent allyl phenol, ortho-phenyl phenol, diphenol, chlorine xylenol etc ( FIG. 1) 。
but natural phenol has far can't satisfy people's needs, and extraction of zhengzhou days began by adopting the method of chemical synthesis of phenol. Extract obtained from coal tar phenol in 1843. As an important basic organic chemical raw materials, phenol has a wide range of USES in the industry, demand is big. In 2006, the total demand to phenol in China reached 780000 t. At home and abroad for many years, is committed to research and explore high selectively direct catalytic synthesis of phenol method and way, and made great progress. Currently, phenol synthesis process is no waste, less waste, high utilization rate of the direction of development. Great concern of the people is the one-step synthesis of phenol. For example, using transition metal vanadium, platinum and tungsten oxide as a catalyst for direct catalytic oxidation of benzene to phenol.
in this paper, using benzene boric acid as raw material, under the condition of copper catalyst, it directly into phenol. Just one can get the goods from the raw material in chemical reaction, in line with the opinions of green synthesis.
liquid-liquid extraction technology in pesticide intermediates phenol synthesis test
benzene boric acid is added to tubular reactor in 1 tendency, CuO10 % tendency, TBAOH 4 tendency. Anaerobic pretreatment on the vacuum tube line: vacuum tube recanalization after 15 min into hydrogen, repeat for 3 times. Fully discharge air, under the condition of the drum of hydrogen, to add 1 mL of methanol reactor. After the completion of feeding, closed reactor, under magnetic stirring, oil bath heated to the required temperature. After the reaction, reaction pipe cooling, add 2 moL/L HCl 15 mL, fully oscillation. Taking the upper organic solution, using method of TLC and silica gel column chromatography separation products and calculate the production rate.
expand reaction. The same reaction system and operation, the use of derivatives of the benzene boric acid as the substrate for reaction, also use the same method to separate the product after the reaction, the yield of the reaction gas chromatograph to determine, using nuclear magnetic resonance (NMR) spectrometer and nuclear magnetic resonance (NMR) analysis of product structure.
liquid-liquid extraction technology in pesticide intermediates phenol synthesis test results and analysis of the
the figure 3 shows that the model reaction yield is very good, is 90%. Homologous derivatives in this reaction system also has good yield, specific results are as follows: when the derivatives of the R group in or between the matchups, reaction yield is generally higher than that of R group at ortho derivative production rate. Thus, the yield of the reaction is affected by the spatial effect of substrates and change. But this does not affect the effect of the system as a whole, the average reaction yield is still high.
liquid-liquid extraction technology in pesticide intermediates phenol synthesis test conclusion and discussion
the test results show that the established effective reaction system has realized the benzene boric acid to the catalytic conversion of phenol; And use of copper catalyst, compared with other precious metal catalyst has the advantage of low price. At the same time, many of phenol derivatives are commonly used pesticide active ingredients, so the test set up reaction system has a strong practical value.
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