A system and method for continuously synthesizing mononitrotoluene in an ultrasonic microreactor

A technology of mononitrotoluene and micro-reactor, which is applied in the field of ultrasonic application and micro-chemical technology, can solve the problems of difficult control of reaction temperature, long reaction time, low safety of mononitrotoluene, etc., and achieve free disassembly and replacement , high heat and mass transfer rate, easy to integrate and scale up

Active Publication Date: 2021-02-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the defects of low safety, uneasy control of reaction temperature and long reaction time in the preparation of mononitrotoluene in the tank reactor, the invention provides a method for continuously synthesizing mononitrotoluene by using an ultrasonic microreactor

Method used

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  • A system and method for continuously synthesizing mononitrotoluene in an ultrasonic microreactor
  • A system and method for continuously synthesizing mononitrotoluene in an ultrasonic microreactor
  • A system and method for continuously synthesizing mononitrotoluene in an ultrasonic microreactor

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Embodiment 1

[0044] In this embodiment, a modular temperature-controlled ultrasonic microreactor with a resonant frequency of 20 kilohertz is used as an example. figure 1 , 3 It can be seen that the ultrasonic microreactor in this embodiment is composed of a sandwich ultrasonic transducer 1.1, a temperature control chamber 1.2, a packaging cover plate 1.3 and a capillary microreactor 3.1.

[0045] The capillary microreactor 3.1 of this embodiment is made of 316 stainless steel, with an outer diameter of 1.6 mm and an inner diameter of 0.6 mm. The sandwich ultrasonic transducer 1.1 has an operating frequency of 20 kHz and a maximum input power of 100W. It consists of a front cover 2.1, a piezoelectric ceramic stack 2.2 and a rear cover 2.3 connected at the center by high-strength metal bolts. The piezoelectric ceramic stack 2.2 is composed of two piezoelectric ceramic sheets stacked coaxially to form a cylinder with a thickness of 10mm. Each piezoelectric ceramic sheet has a thickness of 5...

Embodiment 2

[0047] In this embodiment, a temperature-controlled ultrasonic microreactor with a resonant frequency of 40 kilohertz is used as an example. figure 1 , 3 It can be seen that the ultrasonic microreactor in this embodiment is composed of a sandwich ultrasonic transducer 1.1, a temperature control chamber 1.2, a packaging cover plate 1.3 and a microreactor 3.1.

[0048] The microreactor 3.1 of this embodiment is made of PTFE, with an outer diameter of 2.0 mm and an inner diameter of 1.0 mm. The sandwich ultrasonic transducer 1.1 has an operating frequency of 40 kHz and a maximum input power of 60 W. It consists of a front cover 2.1, a piezoelectric ceramic stack 2.2 and a rear cover 2.3 connected at the center by high-strength metal bolts. The piezoelectric ceramic stack 2.2 is composed of two piezoelectric ceramic sheets coaxially stacked into a cylinder with a thickness of 10mm. The thickness of each piezoelectric ceramic sheet is 5mm and the diameter is 38mm. The piezoelectri...

Embodiment 3

[0050] The temperature-controlled ultrasonic microreactor is the same as example 1, with pure toluene as raw material 1, nitric acid mixed acid as nitrating agent 2 (water 10%, sulfuric acid 68%, nitric acid 22%, mass fraction), utilizes advection pump 3,4 to transport two strands Feed to micromixer and capillary microreactor. The flow rate of toluene is 0.2 ml / min, the flow rate of nitrating agent is 0.3 ml / min, and the ratio of feed material of nitrating agent to toluene is 1.05. The microreactor (with an inner diameter of 0.6 mm) is made of stainless steel, immersed in the ultrasonic radiation area, and the temperature is controlled at 45° C. using a water bath. The ultrasonic radiation frequency is 20KHz, the power is 50W, and the material residence time is 13.2s. The product is collected into the sample collection tank at the outlet, left to stand for phase separation, and the upper organic phase is taken and washed three times with saturated sodium bicarbonate solution ...

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Abstract

A system and method for continuously synthesizing mononitrotoluene in an ultrasonic microreactor. Pure toluene is used as a raw material, and a mixed acid of fuming nitric acid and concentrated sulfuric acid is used as a nitrating agent, and the two are mixed in a microreactor through continuous conveying equipment. , while applying ultrasound of a specific frequency and power. Ultrasonic cavitation causes violent disturbance in the fluid, which can strengthen the mixing between fluids and increase the yield of mononitrotoluene. The temperature of the reaction mixture is controlled at 0-60°C, and the reaction residence time is 2-30s. The invention shortens the synthesis reaction time of mononitrotoluene (the prior art is 10-40min), realizes continuous production, and is easy to integrate and parallel enlargement.

Description

technical field [0001] The invention belongs to the fields of microchemical technology and ultrasonic application, in particular to a method for rapidly synthesizing mononitrotoluene in a microreactor by using ultrasonic waves. Background technique [0002] Mononitrotoluene is an intermediate for large-scale industrial production of fine chemical products such as pesticides, dyes, and pharmaceuticals. Mononitrotoluene is mainly prepared by nitration of toluene, and the nitrating agents used mainly include nitric acid, nitric sulfur mixed acid, nitrogen oxides and organic nitrating agents. Nitrosulfur mixed acid has been used as the main means of nitrating toluene because of its strong nitrifying ability and low price. The mixed acid nitration process of toluene is: toluene diffuses into the mixed acid and is absorbed by the nitronium ions (NO 2 + ) attack, the product nitrotoluene is produced and diffuses back into the organic phase. Because the nitration reaction rate o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/06C07C201/08B01J19/00
CPCB01J19/0093C07C201/08C07C205/06
Inventor 陈光文赵帅南焦凤军温正慧
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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