Method for pipelined continuous production of acetanilide
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A technology of acetanilide and pipeline, which is applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve problems such as slow reaction speed, and achieve small back-mixing, wide source of raw materials, and small online reaction volume Effect
Inactive Publication Date: 2019-06-21
ZHEJIANG UNIV
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The yield of this method is considerable, but the reaction speed is slow
Method used
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Embodiment 1
[0054] Embodiment 1, a kind of method for pipelined continuous production of acetanilide, adopts figure 1 The shown device, with ethyl acetate and aniline as raw material, carries out the following steps successively:
[0055] 1) Add 300 mL of ethyl acetate to measuring cylinder 1, fully open the valves (needle valves 11-13, valve 14) in the system, and use a large flow rate of 10 mL / min to fill the reaction coil 4 with ethyl acetate; put the measuring cylinder Recover the remaining ethyl acetate in 1, then add the reaction raw material---450mL of the mixed solution of ethyl acetate and aniline in graduated cylinder 1, in the mixed solution, the molar ratio of ethyl acetate and aniline is 1:1.
[0056] 2), charge the internal pressure of the system to 3MPa with nitrogen (at this moment, the readings of pressure gauge 8 and pressure gauge 9 are both 3MPa), and close valve 14. Turn on the oil bath 3, set the temperature to 150° C., turn on the heating belt heating device, and m...
Embodiment 2
[0067] Embodiment 2, a kind of method for pipelined continuous production of acetanilide,
[0068] In step 2), the set temperature is 165°C;
[0069] The rest are equal to Example 1.
[0070] Under different flow rate conditions, the reaction yields are shown in Table 2 below:
[0071] Table 2, 165 ℃, raw material ratio 1:1 reaction results
[0072]
Embodiment 3
[0073] Embodiment 3, a kind of method for pipelined continuous production of acetanilide,
[0074] In step 2), the set temperature is 180°C;
[0075] In step 3), set the flow rate at plunger pump 2 to 0.40-1.00mL / min,
[0076] The rest are equal to Example 1.
[0077] Under different flow rate conditions, the reaction yields are shown in Table 3 below:
[0078] Table 3, 180 ℃, raw material ratio 1:1 reaction results
[0079]
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Abstract
The invention discloses a channelized continuous production method of acetanilide. A channelized reaction production device used in the method comprises a reaction coil, wherein the outlet of the reaction coil is connected with the inlet of a high-pressure tank; and a valve is arranged at the outlet of the high-pressure tank. The method comprises the following steps: (1) filling the reaction coil with acetates; (2) pressurizing the reaction coil with inert gas to 3+ / -0.2MPa, and regulating the temperature in the reaction coil to be 150-180 DEG C; (3) reacting a mixed solution of acetates and aniline serving as the reaction raw material in the reaction coil at a certain flow rate, flowing the reacting solution into the high-pressure tank, opening the valve to discharge the reacting solution in the high-pressure tank when the pressure in the high-pressure tank is higher than 5MPa, and closing the valve when the pressure in the high-pressure tank is reduced to be the same as that in the reaction coil set in the step (2); and (4) distilling the reacting solution to remove unreacted raw materials and alcohol serving as a product to obtain the acetanilide.
Description
technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for pipelined continuous production of acetanilide. Background technique [0002] Acetanilide (CAS: 103-84-4), whose molecular formula is C 8 h 9 NO, the relative molecular mass is 135.16, and the molecular structure is as follows: [0003] [0004] Acetanilide, commonly known as antipyretic ice, is an important organic synthesis intermediate of amides, and it can also be used as an analgesic, antipyretic, preservative, rubber and synthetic fiber additive, hydrogen peroxide stabilizer, etc. [0005] The following production methods are currently reported: [0006] Method 1: Zhang Zhang, Li Kanglan, Bai Lin, Journal of Gansu Higher Normal University, 2010, 15(5): 16-18 told four methods of reacting aniline and excess glacial acetic acid to form acetanilide under the catalysis of zinc powder; respectively, fractional distillation , reflux method, reflux-drying method,...
Claims
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