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Device and method for continuously synthesizing o-aminobenzeneethanol by microreactor method

A technology of microreactor and o-aminobenzene, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve unfavorable process scale, continuous production, expensive catalysts, increased production costs, etc. problems, to achieve the effect of good product quality, low production cost and high production efficiency

Active Publication Date: 2015-06-24
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the existing reports, the organic quaternary ammonium base Triton B is used as a catalyst in the hydroxymethylation reaction. Although the reaction can obtain a higher conversion rate, this catalyst is expensive and increases the production cost; zinc can be used in the hydrogenation reaction. Powder reduction method, but this method will cause serious problems such as three wastes; in addition, the traditional batch production process can also be used in the catalytic hydrogenation stage of o-nitrophenylethanol, but this method has high reaction temperature, long production cycle, and hydrogen consumption. The amount is large, and a large amount of organic solvent is required, which is not conducive to the large-scale and continuous production of the process
[0004] At present, various methods for producing o-aminophenylethanol still have disadvantages such as low production efficiency, high cost, and serious wastes. Therefore, we are looking for a green process for o-aminophenylethyl alcohol with continuous reaction, high yield, good quality, low cost, and little environmental pollution. still have important industrial value

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  • Device and method for continuously synthesizing o-aminobenzeneethanol by microreactor method
  • Device and method for continuously synthesizing o-aminobenzeneethanol by microreactor method

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Experimental program
Comparison scheme
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Embodiment 1

[0037] refer to figure 1 , a device for continuously synthesizing o-aminophenethyl alcohol with a microreactor method, comprising a jet mixer 1, a first microreactor 2, a second microreactor 3 and a product collection tank 4 connected in sequence, the jet The inlet end of mixer 1 communicates with the first component tank 5 and the second component tank 6 respectively, and the outlet port of jet mixer 1 communicates with the inlet end of the first microreactor 2, and the first microreactor 2 The outlet port of the second microreactor 3 is communicated with the inlet port of the second microreactor 3, and the outlet port of the second microreactor 3 is communicated with the product collection tank 4, and the inlet port of the second microreactor 3 is also connected with the gas distributor 7 connected.

[0038] The first component tank 5 communicates with the jet mixer 1 through the first metering pump 8, and the second component tank 6 communicates with the jet mixer 1 throug...

Embodiment 2

[0041] refer to figure 1 , a kind of micro-reactor method continuously synthesizes the method for anthranilol, comprises the steps:

[0042](1) Thoroughly mix 57.2g of 2-chloro-6-nitrotoluene and 13ml of dimethyl sulfoxide as the first component, and place it in the first component tank 5; mix 10g of paraformaldehyde, 0.457g of hydrogen Sodium oxide was dissolved in 37ml of methanol as the second component, placed in the second component tank 6. The first component in the first component tank 5 and the second component in the second component tank 6 are simultaneously input into the T-type jet mixer 1 by corresponding first metering pump 8 and second metering pump 9 Mixed, then enter the first microreactor 2 for hydroxymethylation reaction, the first microreactor diameter is 5mm, the length of the tube is 1m, the reaction temperature is controlled at 62°C, and the residence time is 22s to obtain 2-chloro-6-nitro A mixture of phenylethyl alcohol, sodium hydroxide and polar so...

Embodiment 3

[0046] Thoroughly mix 28.6g of 2-chloro-6-nitrotoluene and 6mL of dimethylsulfoxide as the first component; dissolve 5.5g of paraformaldehyde and 0.22g of sodium hydroxide in 19ml of methanol as the second component . The first component and the second component are simultaneously input into the T-shaped jet mixer for rapid mixing, and then enter the first microreactor for methylolation reaction, with a pipe diameter of 5mm and a pipe length of 1.5m, and the reaction temperature is controlled at 65 ℃, residence time 25s, obtain the mixture of 2-chloro-6-nitrophenylethanol, sodium hydroxide and polar solvent; The second microreaction that this mixture is loaded with 40 order Raney nickel catalysts by booster pump At the same time, hydrogen is continuously fed into the reactor through the gas distributor for catalytic hydrogenation. The second microreactor has a pipe diameter of 6mm, a pipe length of 10m, a reaction temperature of 62°C, a reaction pressure of 1.2MPa, and a resid...

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Abstract

The invention relates to a device and a method for continuously synthesizing o-aminobenzeneethanol by a microreactor method. The method comprises the following steps: feeding reactants (2-chloro-6-nitrotoluene and formaldehyde) into a first microreactor and carrying out hydroxymethylation reaction at a certain temperature in the presence of an alkali serving as a catalyst in a polar solvent serving as a carrier so as to obtain a mixture of 2-chloro-6-nitrophenethyl alcohol and the polar solvent; and feeding the mixture into a second microreactor and continuously feeding hydrogen gas by a gas distributor at the same time so as to carry out catalytic hydrogenation, thus obtaining o-aminobenzeneethanol, wherein the second microreactor is loaded with a hydrogenation catalyst. According to the method, cheap raw materials and catalysts are used, a proper temperature is selected, and the continuous production is realized by virtue of the microreactors. The method has the advantages of high production efficiency, easy control over reaction conditions, high product yield, high product quality and full utilization of resources and therefore is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a device and a method for continuously synthesizing o-aminophenethyl alcohol with a microreactor method. Background technique [0002] Anthranilol is an important basic raw material for fine chemicals, widely used in medicine, pesticides, spices, food and feed additives, dyes and other fields. The research on its application has been persistent, and new application fields are still being developed. . [0003] At present, the synthesis technology of o-aminophenylethanol that has been industrialized is mainly prepared from o-nitrotoluene through methylolation and hydrogenation. In the existing reports, the organic quaternary ammonium base Triton B is used as a catalyst in the hydroxymethylation reaction. Although the reaction can obtain a higher conversion rate, this catalyst is expensive and increases the production cost; zinc can be used in the hydrogenation reaction. Powder reduction method, but this method will cause seriou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/68C07C213/02
Inventor 秦振伟肖庆军潘志军施云龙陈国泉徐怡清
Owner ZHEJIANG DINGLONG TECH