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Method for synthesizing acyl naphthalene by using micro-channel reactor

A microchannel reactor and reactor technology, applied in the direction of condensation preparation of carbonyl compounds, separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of long reaction time, low product yield, and no mention of product purification, etc. To achieve the effect of short material residence time, reduce reaction time, and increase reaction kinetic rate

Inactive Publication Date: 2018-04-06
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY +1
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  • Abstract
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Problems solved by technology

[0004] CN100334058C (2007-08-29) patent has introduced the method that 2-alkyl naphthalene is prepared 2-alkyl-6-acyl naphthalene by Friedel–Crafts reaction, and this reaction is batch reaction, and reaction time is longer, and product yield is lower , and did not mention how to purify the product
[0005] CN101270040B (2011-06-22) patent introduces a production method of 6-methoxy-2-acetyl, the reaction is a batch reaction, the reaction time is long, and only a single Lower alcohols, although the purity of the product is improved but the yield of the product is low

Method used

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  • Method for synthesizing acyl naphthalene by using micro-channel reactor

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Experimental program
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Embodiment 1

[0020] Put the stirred reactor into a low-temperature tank, add 15g of nitrobenzene, then add 2.5g of anhydrous aluminum trichloride, and finally add 1.3g of propionyl chloride, control the temperature at 0°C, and react for 10 minutes to prepare acylation liquid. Add 15g of nitrobenzene into a stirred reactor, and then add 1.5g of 2-methylnaphthalene to prepare a raw material solution. Use a metering pump to draw the raw material liquid and the acylation liquid respectively, inject the two materials into a T-shaped mixer through a syringe for mixing, and then enter the microchannel reactor (inner diameter 0.5mm, length 6m) for reaction, the reaction time is 60min, where T The type mixer is placed in a constant temperature tank to control the temperature at 0°C, and the reaction tube is placed in the constant temperature tank to control the temperature at 35°C. The reacted product enters the T-type mixer again, and the other water is injected into the mixer through the meterin...

Embodiment 2

[0022] Put the stirred reactor into a low-temperature tank, add 15g of nitrobenzene, then add 4.5g of anhydrous aluminum trichloride, and finally add 2.5g of propionic anhydride, control the temperature at 0°C, and react for 10 minutes to prepare acylation liquid. Add 15g of nitrobenzene into a stirred reactor, and then add 1.5g of 2-methylnaphthalene to prepare a raw material solution. Use a metering pump to draw the raw material liquid and the acylation liquid respectively, inject the two materials into a T-shaped mixer through a syringe for mixing, and then enter the microchannel reactor (inner diameter 0.5mm, length 6m) for reaction, the reaction time is 60min, where T The type mixer is placed in a constant temperature tank to control the temperature at 0°C, and the reaction tube is placed in the constant temperature tank to control the temperature at 35°C. The reacted product enters the T-type mixer again, and the other water is injected into the mixer through the meteri...

Embodiment 3

[0024] Put the stirred reactor into a low-temperature tank, add 15g of nitrobenzene, then add 2.5g of anhydrous aluminum trichloride, and finally add 1.2g of acetyl chloride, control the temperature at 0°C, and react for 10 minutes to prepare acylation liquid. Add 15g of nitrobenzene into a stirred reactor, and then add 1.5g of 2-methylnaphthalene to prepare a raw material solution. Use a metering pump to draw the raw material liquid and the acylation liquid respectively, inject the two materials into a T-shaped mixer through a syringe for mixing, and then enter the microchannel reactor (inner diameter 0.5mm, length 6m) for reaction, the reaction time is 60min, where T The type mixer is placed in a constant temperature tank to control the temperature at 0°C, and the reaction tube is placed in the constant temperature tank to control the temperature at 35°C. The reacted product enters the T-type mixer again, another water is injected into the mixer through the metering pump, a...

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Abstract

The invention discloses a method for synthesizing acyl naphthalene by using a micro-channel reactor. The method comprises the following steps: (1) preparing acylation liquid, namely adding nitrobenzene and anhydrous aluminum chloride into a reactor in a low-temperature tank, finally adding acyl chloride, and controlling the temperature in the reactor to be 0-3 DEG C; (2) preparing a feed solution,namely adding nitrobenzene and 2-methyl naphthalene into a reactor provided with a stirrer; (3) reacting, namely injecting the feed solution and the acylation liquid into a micro mixer to be mixed, and feeding into the micro-channel reactor to be reacted; (4) washing, namely enabling the product discharged from the micro-channel reactor to enter the micro mixer again so as to be washed, enablingthe mixture into the micro-channel reactor, controlling the reactor temperature to 40-50 DEG C, and performing ultrasonic oscillation outside the reactor; (5) performing reduced pressure distillation,namely separating the products obtained in the step (4), and performing vacuum decompression to 500-1000Pa so as to obtain a crude product 2-methyl-6-acyl naphthalene; and (6) recrystallizing, namelyadding the crude product obtained in the step (5) into a solvent of 50-60 DEG C, stirring and dissolving, naturally cooling and crystallizing, continuously cooling and crystallizing in an ice-water bath, and finally filtering to obtain the purified product 2-methyl-6-acyl naphthalene.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing acylnaphthalene using a microchannel reactor. Background technique [0002] 2,6-naphthalene dicarboxylic acid is an important chemical intermediate for the preparation of polyethylene naphthalate, and 2-methyl-6-acylnaphthalene is an important raw material for the preparation of 2,6-naphthalene dicarboxylic acid, 2-methyl Naphthalene is cheap and easy to obtain, so it is very meaningful to prepare 2-methyl-6-acylnaphthalene by using 2-methylnaphthalene as raw material through Friedel–Crafts reaction. [0003] At present, Mitsubishi Gas Chemical Company of Japan has used 2-methylnaphthalene as the reaction raw material, acetyl fluoride as the acylating agent, and HF / BF 3 As a catalyst, 2-methyl 6-acetylnaphthalene was prepared by acylation under the conditions of temperature 35°C and pressure 2.0 MPa. Although this method has the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C45/78C07C45/80C07C45/81C07C49/788
CPCC07C45/46C07C45/78C07C45/80C07C45/81C07C49/788
Inventor 靳海波李文鹏郭学华杨索和何广湘郭晓燕杨大志王亚涛
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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