Process and device for continuously producing bentazone intermediate o-aminobenzoic acid

A technology of isopropylamine anthranilic acid and isopropylamine anthranilic acid is applied in the field of continuous production of anthranilic acid, an intermediate of bentazone, and can solve the problem of excessive waste organic solvents and low productivity. problem, to achieve the effect of large reaction heat transfer coefficient, low cost and reduced production cost

Active Publication Date: 2021-01-01
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly aims at the problems of low existing productivity and many waste organic solvents, and provides a continuous production of bentazone intermediate o-aminobenzene that can realize continuous production, product quality, stable performance, low energy consumption and no waste organic solvents. Process and device for isopropylamine formate

Method used

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  • Process and device for continuously producing bentazone intermediate o-aminobenzoic acid

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Experimental program
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Effect test

Embodiment 1

[0032] A kind of technique of continuous production of isopropylamine anthranilate is realized by following device:

[0033] Described phthalimide 1 bottom is connected with the middle part of microchannel reactor 3 by pipeline a, and the bottom of sodium hypochlorite storage tank 2 is connected with the middle part of microchannel reactor 3 by pipeline b, and described microchannel device The bottom of 3 is connected to the upper part of the temporary storage tank 4 through the pipeline c, the bottom of the temporary storage tank 4 is connected to the upper part of the static mixer 6 through the pump and the pipeline d, and the bottom of the hydrochloric acid storage tank 5 is connected through the pipeline e Be connected with the top of static mixer 6, the bottom of described static mixer 6 is connected with isopropylamine anthranilic acid reaction kettle 7 tops by pipeline f, the bottom of described isopropylamine aqueous solution stirring tank 8 is passed pipeline g Link t...

Embodiment 2

[0038] (1) Add 200kg of phthalimide, 600kg of pure water, and 187kg of 32% sodium hydroxide solution to phthalimide alkalization reaction kettle 1, start stirring, control the stirring level at 6, and turn on the regulating motor The rotating speed makes the material reach a turbulent state, the material gradually dissolves, and the solution is clarified;

[0039] (2) Phthalimide alkalization reactor 1, sodium hypochlorite (available chlorine mass content is 8%) storage tank 2 opens corresponding bottom valve, through the interlocking control of flow meter and valve, according to sodium hypochlorite and adjacent The phthalamide molar ratio of 1.2:1 enters the microchannel reactor 3, and the feed direction of the phthalimide alkalization solution forms a 90° angle with the feed direction of the sodium hypochlorite solution and opens the refrigerant valve of the reactor, The temperature of the control solution is -15°C, and the generated solution enters the temporary storage tan...

Embodiment 3

[0045] (1) Add 200kg of phthalimide, 1000kg of pure water, and 204kg of 32% sodium hydroxide solution to phthalimide alkalization reaction kettle 1, start stirring, control the stirring level at 8, and turn on the regulating motor The rotating speed makes the material reach a turbulent state, the material gradually dissolves, and the solution is clarified;

[0046] (2) Phthalimide alkalization reaction kettle 1, sodium hypochlorite (available chlorine mass content is 13%) storage tank 2 opens corresponding bottom valve, through the interlocking control of flowmeter and valve, according to sodium hypochlorite and adjacent The phthalamide molar ratio of 1.1:1 enters the microchannel reactor 3, and the feeding direction of the phthalimide alkalization solution forms an angle of 100° with the feeding direction of the sodium hypochlorite solution, and the refrigerant valve of the reactor is opened. The temperature of the control solution is -20°C, and the generated solution enters ...

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Abstract

The invention discloses a process and a device for continuously producing bentazone intermediate o-aminobenzoic acid isopropyl amine by taking phthalimide as a raw material. The process comprises thefollowing steps: (1) adding phthalimide solid and pure water into a reaction kettle, stirring at a low speed, adding a 32% sodium hydroxide solution, and stirring at normal temperature for 30 minutes;(2) respectively feeding the phthalimide sodium salt solution and the sodium hypochlorite solution into a micro-channel reactor according to a certain flow rate, carrying out a Huffman rearrangementreaction at a low temperature, and feeding the mixture into a temporary storage tank; (4) mixing the reaction solution in the temporary storage tank 1 with hydrochloric acid (or sulfuric acid and thelike) through a static mixer, feeding the mixture into a reaction kettle, heating the mixture to room temperature, adding an isopropylamine aqueous solution at a certain flow rate, and continuously stirring for 2-3 hours; (4) enabling the solution to pass through a plate-and-frame filter press, returning the filtrate to the first step for repeated application, and drying the filter cake to obtainisatoic anhydride with the purity of 99% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical equipment, and in particular relates to a process and a device for continuously producing bentazone intermediate anthranilic acid. [0002] technical background [0003] Bentazon is a systemic conduction herbicide successfully developed by Baden Company in Germany in 1968. It is suitable for various crops such as rice, wheat, corn, soybean, peanut, pea, alfalfa and poisonous weeds in pastures, and has excellent control effect on broad-leaved weeds and sedge weeds. Bentazon has the advantages of high efficiency, low toxicity, wide herbicidal spectrum, no phytotoxicity, and good compatibility with other herbicides, so it is in great demand. Propylamine demand also increased sharply. [0004] Since the rise of micro-reaction technology in the mid-1990s, the research and application of micro-channel reactors have attracted extensive attention from researchers at home and abroad, and have been increa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/10C07C237/30B01J19/00
CPCC07C231/10B01J19/0093C07C237/30
Inventor 岳涛郭鹏王达彤徐婷卢福军
Owner QINGDAO UNIV OF SCI & TECH
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