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A kind of continuous synthesis 2, the method for 4-dinitroanisole

A technology of dinitroanisole and dinitrochlorobenzene, applied in the field of continuous chemical synthesis, can solve the problems of long cycle, large amount of waste water, high cost, etc., and achieve low pollution, low cost, safe and reliable process Effect

Active Publication Date: 2019-01-15
HUBEI DONGFANG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems such as high cost, long cycle and large amount of waste water that cannot be continuously caused by 2,4-dinitroanisole (DNAN) products, and provide a continuous, short synthesis cycle and low production cost. , 2,4-dinitroanisole (DNAN) industrial synthesis method with little amount of waste water

Method used

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  • A kind of continuous synthesis 2, the method for 4-dinitroanisole

Examples

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Effect test

Embodiment 1

[0022] (1) 2,4-dinitrochlorobenzene (CDB) in a molten state at 65°C, methanol at 20°C and 30% liquid caustic soda solution with a mass fraction of 20°C are continuously added to the In the reactor, keep the temperature in the reactor constant at 65°C;

[0023] (2) The synthetic reaction solution enters the evaporator continuously, and the methanol enters the rectification tower from the vapor phase outlet of the evaporator, and from the top of the rectification tower to the recovery bottle, it contains 2,4-dinitroanisole (DNAN), chlorinated The sodium aqueous solution enters the washing tank continuously from the liquid phase outlet of the evaporator;

[0024] (3) After being washed with hot water at 95°C in the washing tank, it enters the separator for static separation, and the separated wastewater is collected for unified treatment. The product 2,4-dinitroanisole (DNAN) is collected and then dried, weighed, analysis test;

[0025] Through analysis and testing, it was foun...

Embodiment 2

[0027] (1) Continuously transport methanol, liquid caustic soda, and molten 2,4-dinitrochlorobenzene (CDB) to corresponding raw material head tanks respectively;

[0028] (2) The lye, methanol and 2,4-dinitrochlorobenzene (CDB) are continuously added to the reactor from the head tank at a mass ratio of 1:0.72:5, and the temperature of the reactor is set at 65°C under normal pressure. , the reaction liquid enters the curing machine continuously through the lifting system of the reactor, and the setting temperature of the curing machine is 65°C and normal pressure;

[0029] (3) The mixed material in the aging machine enters the evaporator continuously through the lifting system, and the evaporator adopts a tank-type self-circulation mode, and the reaction liquid after removing methanol continuously enters the first washing tank from the side of the evaporator, and the evaporator evaporates Methanol and water vapor continuously enter the methanol rectification tower. The tower is...

Embodiment 3

[0035] (1) Continuously transport methanol, liquid caustic soda, and molten 2,4-dinitrochlorobenzene (CDB) to corresponding raw material head tanks respectively;

[0036] (2) Lye, methanol and 2,4-dinitrochlorobenzene (CDB) are continuously added to the reaction kettle from the head tank at a mass ratio of 1:0.72:8, and the reaction kettle is set at a temperature of 62°C and normal pressure , the reaction liquid enters the curing machine continuously through the lifting system of the reactor, and the setting temperature of the curing machine is 62°C and normal pressure;

[0037] (3) The mixed material in the aging machine enters the evaporator continuously through the lifting system, and the evaporator adopts a tank-type self-circulation mode, and the reaction liquid after removing methanol continuously enters the first washing tank from the side of the evaporator, and the evaporator evaporates Methanol and water vapor continuously enter the methanol rectification tower. The t...

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Abstract

The invention discloses a method for continuously synthesizing 2,4-dimitroanisole, and relates to the field of synthesis of chemical raw materials. The method mainly comprises the following five steps of synthesis, recovery of methyl alcohol, washing, drying, and flaking and packaging. The method has the advantages that by adopting the continuous synthesis method, the recovery rate of solvent is high, the pollution is little, the cost is low, and the safety, reliability and stability are realized in the process; the total yield of product is more than 90%, and the purity is more than 99.2%.

Description

technical field [0001] The invention relates to the field of chemical raw material synthesis, in particular to a method for continuously synthesizing 2,4-dinitroanisole. Background technique [0002] 2,4-Dinitroanisole (DNAN) is a newly reported carrier of melt-cast explosives with excellent performance. The molecular formula is C7H6N3O5, the density is 1.341g / cm3, a bright brown to light yellow crystalline solid, slightly soluble in water, soluble in most organic solvents, including methanol, ethanol, and ether. [0003] In 2015, Zhejiang Dibang Chemical Co., Ltd. declared and authorized an invention patent authorization of "a synthesis process of 2,4-dinitroanisole", the patent number is CN201310325839.8. The synthesis method of 2,4-dinitroanisole mentioned in this patent is to dissolve the composite inorganic base in methanol to obtain methanol lye, and then add the methanol lye dropwise to CDB to carry out the synthesis reaction, and the reaction liquid cools down to cr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/12C07C205/37
CPCC07C201/12C07C205/37
Inventor 方克雄魏伍山陈军潘红霞龚磊赵勤常雯宇刘学云姚中英
Owner HUBEI DONGFANG CHEM IND
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