Method for continuously producing resorcin

A technology of resorcinol and m-phenylenediamine, which is applied in the field of continuous production of resorcinol in a loop reaction device, can solve the problems of high control requirements of production equipment and operation process, small production capacity per unit volume of equipment and poor product quality. Stability and other problems, to achieve the effect of solving the uneven temperature distribution of the material, solving the back mixing of the material, and being easy to control

Active Publication Date: 2014-07-23
淮安嘉诚高新化工股份有限公司
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AI Technical Summary

Problems solved by technology

At present, the commonly used nitrification process is the traditional isothermal multi-tank series nitrification and adiabatic nitrification process. Due to the fast nitrification reaction speed and strong exothermic reaction process, there are certain safety hazards in the production process, especially the dinitrification process, which has great impact on production equipment and operation process. higher control requirements
At present, the hydrogenation reduction of dinitrobenzene to produce m-phenylenediamine mainly adopts the batch reaction. The disadvantages of this process are: high production cost, high labor intensity, poor operating environment, unstable product quality, and the unit volume capacity of the equipment. Small, large investment in equipment, etc.

Method used

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  • Method for continuously producing resorcin
  • Method for continuously producing resorcin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: as figure 1 Shown to produce resorcinol

[0029] (1) Preparation of dinitrobenzene by nitration of benzene: The mixed acid containing 70% sulfuric acid, 10% nitric acid, and 20% water is continuously sent to the static mixer together with benzene, and then enters the nitration microchannel reactor for adiabatic nitration reaction , the molar feeding ratio of nitric acid and benzene is 2:1.05, the nitrification temperature is controlled at 120°C, the residence time of the reaction material is 1s, the nitrification liquid enters the separator continuously, and the waste acid is separated to obtain crude dinitrobenzene, and the waste acid is dehydrated by flash evaporation Remove the waste acid storage tank, then use fresh benzene to extract and treat it, and then denitrify the reactor for recycling. The crude product of dinitrobenzene is neutralized, dephenolized, washed and refined to obtain dinitrobenzene, and the yield of dinitrobenzene is 99.1 %, the pu...

Embodiment 2

[0032] Embodiment 2: as figure 1 Shown to produce resorcinol

[0033] (1) Preparation of dinitrobenzene by nitration of benzene: (1) Preparation of dinitrobenzene by nitration of benzene: The mixed acid containing 77% sulfuric acid, 8% nitric acid and 15% water is continuously fed into the static mixer together with benzene, Then enter the nitration microchannel reactor for adiabatic nitration reaction, the molar feeding ratio of nitric acid and benzene is 2:1.13, the nitration temperature is controlled at 150°C, the residence time of the reaction material is 10s, the nitration liquid enters the separator continuously, and the spent acid is separated to obtain The crude product of dinitrobenzene, the waste acid is flashed and dehydrated to the waste acid storage tank, and then extracted with fresh benzene, then the denitration reactor is recycled, and the crude product of dinitrobenzene is neutralized, dephenolized, washed and refined to obtain dinitrobenzene The yield of nit...

Embodiment 3

[0036] Embodiment 3: as figure 1 Shown to produce resorcinol

[0037] (1) Preparation of dinitrobenzene by nitration of benzene: (1) Preparation of dinitrobenzene by nitration of benzene: The mixed acid containing 85% sulfuric acid, 10% nitric acid and 5% water is continuously fed into the static mixer together with benzene, Then enter the nitration microchannel reactor for adiabatic nitration reaction, the molar feeding ratio of nitric acid and benzene is 2:1.2, the nitration temperature is controlled at 180°C, the residence time of the reaction material is 20s, the nitration liquid enters the separator continuously, and the waste acid is separated to obtain The crude product of dinitrobenzene, the waste acid is flashed and dehydrated to the waste acid storage tank, and then extracted with fresh benzene, then the denitration reactor is recycled, and the crude product of dinitrobenzene is neutralized, dephenolized, washed and refined to obtain dinitrobenzene The yield of nitr...

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Abstract

The invention discloses a method for continuously producing resorcin. According to the method, benzene serves as a starting raw material, resorcin is continuously produced through three steps, namely benzene nitration, dinitrobenzene hydrogenated reduction and m-phenylenediamine hydrolysis, devices for benzene nitration and m-phenylenediamine hydrolysis are microchannel reactors, and the reaction for preparing m-phenylenediamine through the catalytic hydrogenated reduction of dinitrobenzene adopts a loop reaction device. The method has the advantages that the phenomena of material backmixing and non-uniform material temperature distribution of the conventional reactors are thoroughly solved, the occurrence of side reactions is reduced, the yield of the product is increased, and the quality of the product is improved; the safety of production during nitration and hydrolysis is improved, meanwhile, the waste of reactants is avoided, and environmental pollution is reduced; and the unit volume production capacity of equipment is increased greatly and is increased by 8-10 times compared with that of kettle type equipment, the production process flow is simplified, and the equipment investment is reduced.

Description

technical field [0001] The invention relates to a method for producing resorcinol, in particular to a method for continuously producing resorcinol by using benzene as a starting material, using microchannel reactors for nitration and hydrolysis equipment, and loop reaction devices for hydrogenation reduction equipment. Background technique [0002] Resorcinol, commonly known as resorcinol, is an important fine organic chemical raw material, widely used in agriculture, dyes, coatings, medicine, plastics, rubber, electronic chemicals, etc. -Adhesives and high-performance adhesives for wood plywood, etc. [0003] The currently industrialized resorcinol synthesis methods mainly include: benzene sulfonation alkali fusion method, m-dicumene oxidation method and m-phenylenediamine hydrolysis method. Among them, the m-phenylenediamine hydrolysis method is a new clean production process for the production of resorcinol. The product cost is about 20% to 30% lower than the existing be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C37/05C07C211/51C07C209/36
CPCC07C37/05C07C201/08C07C209/36C07C39/08C07C211/51C07C205/06
Inventor 石祖嘉
Owner 淮安嘉诚高新化工股份有限公司
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