Catalyst for polyfluorinated benzoate reduction preparation of polyfluorinated benzyl alcohol and method thereof
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A technology of polyfluorobenzoic acid and polyfluorobenzyl alcohol is applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., and can solve the problems of low yield, difficult purification, and high cost of sodium borohydride, Achieve the effect of large output, no environmental protection pressure, and easy recycling
Active Publication Date: 2015-08-12
DALIAN QIKAI MEDICAL TECH
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[0007] 2. Zhejiang Zhongxin Chemical Industry, a preparation method of 2,3,4,5,6-pentafluorobenzyl alcohol, CN101412660A: the reaction mechanism is complicated, the reaction selectivity is not good, the purification is difficult, and the yield is low
[0009] 3. East China Normal University, Method for Synthesizing Polyfluorobenzyl Alcohol by Reducing Polyfluorobenzoic Acid with Sodium Borohydride, CN101012148A: This method is simple, but it has defluorination by-products and is not easy to purify
[0011] 4. Jiangsu Yangnong Chemical Co., Ltd., a new process for preparing transfluthrin, CN1631869A, discloses the use of reducing agents and auxiliary agents in solvents by 2,3,5,6-tetrafluorobenzoate Preparation of 2,3,5,6-tetrafluorobenzyl alcohol by reduction, using sodium borohydride as reducing agent, sodium borohydride has high cost and produces a large amount of waste solid inorganic salt
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Embodiment 1
[0037] The preparation of embodiment 1 catalyst
[0038] 10g of copper oxide, 10g of zinc oxide and 83g of aluminum oxide were mixed to obtain a catalyst, and 5g of graphite was added for use.
Embodiment 2
[0039] The preparation of embodiment 2 catalyst
[0040] Mix 50g of copper oxide, 30g of zinc oxide, 5g of cerium oxide and 420g of aluminum oxide to obtain a catalyst, which is ready for use.
Embodiment 3
[0041] The preparation of embodiment 3 catalyst
[0042] 1. Reaction
[0043] Add 235g of copper nitrate, 155g of zinc nitrate, 10g of cerium nitrate, and 65g of aluminum hydroxide to 2000g of pure water, heat to 60-70°C, add 28% ammonia water under stirring, adjust the pH to 7-8 to cause precipitation, and obtain The precipitate is a mixture of copper hydroxide, zinc hydroxide, aluminum hydroxide, and cerium hydroxide.
[0044] 2. Drying
[0045] Filter and wash the filter cake, and dry at 100-110°C for 5-8 hours to remove the precipitation and moisture brought during the filtration process;
[0046] 3. Roasting
[0047] Roast in a muffle furnace at 500-600°C for 4-6 hours to prepare the metal in the hydroxide state into an oxidized state to obtain copper oxide, zinc oxide, cerium oxide and aluminum oxide, and naturally cool down to room temperature;
[0048] 4. Tablet
[0049] 5g of graphite was added to every 100g of powder solids as a binder, and after mixing evenly, ...
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Abstract
The invention discloses a catalyst for polyfluorinated benzoate reduction preparation of polyfluorinated benzyl alcohol; the catalyst includes the components in parts by weight: 10-50 parts of copper oxide, 10-30 parts of zinc oxide, 1-5 parts of cerium oxide, and 10-40 parts of aluminum oxide; graphite is mixed and added in the catalyst, and the catalyst is treated for 20-26 h by introducing hydrogen at the temperature of 170-220 DEG C. The catalyst is used for polyfluorinated benzoate reduction preparation of polyfluorinated benzyl alcohol, and has the advantages of good reaction selectivity, high yield, and easy industrialized production. The invention also provides a method for polyfluorinated benzoate reduction preparation of polyfluorinated benzyl alcohol by using the catalyst; the catalyst is packed in a fixed bed reactor, hydrogen is introduced at the temperature of 200-210 DEG C, the hydrogen pressure is 2.0-2.5 MPa, and the hydrogen flow rate is 1-2 L/min; an alcohol solution of polyfluorinated benzoate is added by a high-pressure metering pump, continuous production can be carried out, the yield is high, a by-product only comprises alcohol and is easy to recycle, no three waste generated by other processes exists, no environmental protection pressure exists, and the polyfluorinated benzyl alcohol yield is greater than 90%.
Description
technical field [0001] The present invention relates to the technical field of fine chemicals, in particular to a catalyst for preparing polyfluorobenzyl alcohol from polyfluorobenzoic acid esters and a method thereof. Background technique [0002] Fluorobenzyl alcohol is an intermediate of Penfluthrin, an insecticidal pesticide with high efficiency and low toxicity. [0003] The existing synthetic routes mainly include: [0004] 1. US patent: US6020517, a process for preparing benzyl alcohol from pentafluorobenzonitrile [0005] The reaction mechanism is complicated, the reaction selectivity is bad, the purification is difficult, and the yield is low. [0006] [0007] 2. Zhejiang Zhongxin Chemical Industry, a preparation method of 2,3,4,5,6-pentafluorobenzyl alcohol, CN101412660A: the reaction mechanism is complicated, the reaction selectivity is not good, the purification is difficult, and the yield is low. [0008] [0009] 3. East China Normal University, Metho...
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