Production method of 3-cyanobenzoic acid
A technology of cyanobenzoic acid and production method, applied in chemical instruments and methods, preparation of carboxylic acid nitrile, preparation of organic compounds, etc., can solve problems such as hidden dangers, troublesome waste water treatment, etc. High rate and purity effect
Inactive Publication Date: 2013-07-24
HUBEI UNIV OF TECH
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Problems solved by technology
Although this method has been industrialized, there are still some problems
The waste water treatment after the reaction is also very troublesome
Moreover, there are certain hidden dangers in the production of highly toxic metal cyanide, which is the biggest problem of this type of reaction.
Method used
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Embodiment 1
[0031] first step, to figure 1 Add 800 liters of 3-methylbenzonitrile to the shown 1000 liter enamel reaction kettle 1 and heat to 150-160° C. Feed liquid is continuously pumped into the top of the enamel packed tower 2 with a pump, and sprayed downward with a flow rate of 15 liters / minute. Simultaneously feed 310 kilograms of chlorine gas equably from the lower part of the packed tower with a flow rate of 15 liters per minute to form 3-methylbenzonitrile and chlorine gas in reverse motion. The gas phase is cooled by the sheet-type enamel condenser 3, separated by the gas-liquid separator 4, and the liquid returns to the enamel reaction kettle. Hydrogen chloride and chlorine gas enter the tail gas absorption tank 5 and are emptied after being absorbed by water and alkali.
[0032] Insulation reaction, in the reaction process, detect the content of 3-chloromethylbenzonitrile in the reactor by gas chromatography at regular intervals, when the content of 3-chloromethylbenzonitr...
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Abstract
The invention relates to a production method of 3-cyanobenzoic acid. The production method comprises the following steps of step 1, reacting 3-cyano toluene as an initial raw material with chlorine gas in a reversed tower-type reactor to generate 3-chloromethyl cyanophenyl; and step 2, carrying out heating oxidation reaction on 3-chloromethyl cyanophenyl through hydrogen peroxide under the effects of vanadyl sulfate and sodium tungstate catalysts and benzyl chloride triethylammonium phase transfer catalyst to generate 3-cyanobenzoic acid, continuing heating and distilling to remove ethanol, cooling to room temperature, filtering, washing the filter cake through water twice, recrystallizing by ethanol and drying to obtain 3-cyanobenzoic acid white powder. The total yield of the product in two steps can reach 80 percent, the content can reach 98 percent, the cost is low, and the production method is applicable to industrialized production. The yield and purity of the product are high, the environmental pollution is small, and the cost is low.
Description
technical field [0001] The present invention relates to a kind of production method of 3-cyanobenzoic acid. Background technique [0002] 3-cyanobenzoic acid is an important intermediate in organic synthesis. It is widely used in the preparation of cardiovascular drugs, antibiotics, analgesics and nervous system regulation drugs, etc., and is also an important raw material for the synthesis of liquid crystal materials. The synthetic method of existing 3-cyanobenzoic acid mainly contains following several kinds: [0003] East China Normal University Yang Fan etc. (CN01105687.8) take 3-cyanotoluene as raw material, divalent cobalt salt as catalyst, sodium bromide as promoter, oxygen in the air as oxidant, prepare 3-cyanobenzoic acid, yield 80-99%. The disadvantage of this method is that the reaction needs to be carried out in a sealed tube, the reaction temperature is high, and the pressure is high. This method is particularly suitable for the preparation of 3-cyanobenzoic...
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IPC IPC(8): C07C255/57C07C253/30
Inventor 徐保明陈坤唐强胡传群阮华屹韩洋洋胡欢张杰裴智山
Owner HUBEI UNIV OF TECH