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Synthesis process of sodium p-nitrophenolate

A technology of sodium p-nitrophenolate and synthesis process, which is applied in the field of fine chemical product synthesis, can solve the problems of excessive temperature and pressure rise, low production efficiency, high labor intensity, etc., and achieves mild reaction, easy handling, and excellent resistance. alkaline effect

Active Publication Date: 2021-08-03
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production efficiency of this process is low, the product yield is low, and a large amount of waste water is produced in the production process, and the labor intensity is high.
[0003]According to thermochemical theory, the hydrolysis reaction of p-nitrochlorobenzene and sodium hydroxide is an exothermic reaction, △H=178KJ / mol, participating in the hydrolysis reaction The concentration of sodium hydroxide should not be too high, because the concentration of alkali is too high to easily produce black material; the concentration of alkali increases, the reaction speed is doubled, a large amount of heat is released instantaneously, and the temperature and pressure in the kettle rise too fast, which is difficult to control. , Sodium p-nitrophenolate generated under alkaline conditions will undergo reduction condensation reaction to form black material phenomenon

Method used

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  • Synthesis process of sodium p-nitrophenolate
  • Synthesis process of sodium p-nitrophenolate
  • Synthesis process of sodium p-nitrophenolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of quaternary ammonium surfactants:

[0030] Step S11, mix sodium sulfite and deionized water to prepare a saturated solution, set the temperature at 85°C, add epichlorohydrin dropwise, and control the dropwise addition time to 1.5h, after the dropwise addition, keep the temperature unchanged, and continue the reaction for 1.5 h, after the reaction, the temperature of the reaction solution was lowered to room temperature, and crystals were precipitated, then filtered under reduced pressure, and recrystallized with deionized water to obtain intermediate 1;

[0031] Step S12, mix xylene and diethylenetriamine, set the temperature to 90°C, add the mixed xylene and diethylenetriamine dropwise to benzoic acid, after the dropwise addition, continue to heat up to 140°C, at this The reaction was continued at low temperature for 3 hours, and then the temperature was raised to 240° C., and the reaction was continued for 3 hours. After the reaction, intermediate 2 was ...

Embodiment 2

[0035] Preparation of quaternary ammonium surfactants:

[0036] Step S11, mix sodium sulfite and deionized water to prepare a saturated solution, set the temperature at 85°C, add epichlorohydrin dropwise, and control the dropwise addition time to 1.8h. After the dropwise addition, keep the temperature unchanged and continue the reaction for 1.5 h, after the reaction, the temperature of the reaction solution was lowered to room temperature, and crystals were precipitated, then filtered under reduced pressure, and recrystallized with deionized water to obtain intermediate 1;

[0037] Step S12, mix xylene and diethylenetriamine, set the temperature to 90°C, add the mixed xylene and diethylenetriamine dropwise to benzoic acid, after the dropwise addition, continue to heat up to 145°C, at this The reaction was continued at low temperature for 3 hours, and then the temperature was raised to 240° C., and the reaction was continued for 3 hours. After the reaction, Intermediate 2 was o...

Embodiment 3

[0041] Preparation of quaternary ammonium surfactants:

[0042] Step S11, mix sodium sulfite and deionized water to prepare a saturated solution, set the temperature at 85°C, add epichlorohydrin dropwise, and control the dropwise addition time to 2h, after the dropwise addition, keep the temperature unchanged, and continue the reaction for 1.5h , after the reaction, the temperature of the reaction solution was lowered to room temperature, crystals were precipitated, then filtered under reduced pressure, and recrystallized with deionized water to obtain intermediate 1;

[0043] Step S12, mix xylene and diethylenetriamine, set the temperature to 90°C, add the mixed xylene and diethylenetriamine dropwise to benzoic acid, after the dropwise addition, continue to heat up to 150°C, at this The reaction was continued at low temperature for 3 hours, and then the temperature was raised to 240° C., and the reaction was continued for 3 hours. After the reaction, intermediate 2 was obtain...

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Abstract

The invention discloses a synthesis process of sodium p-nitrophenolate, and belongs to the technical field of fine chemical product synthesis. The synthesis process comprises the following steps of: 1, introducing nitrogen into a reaction kettle, then preheating the reaction kettle to 160-165 DEG C, controlling the pressure to be 0.75-0.8 MPa, adding a quaternary ammonium salt surfactant into p-nitrochlorobenzene, and preheating p-nitrochlorobenzene and a sodium hydroxide solution to 150-155 DEG C; 2, feeding: during feeding, controlling the flow of p-nitrochlorobenzene to be 600-640g / h and the flow of the sodium hydroxide solution to be 5100-5200g / h; and 3, cooling and crystallizing the obtained reaction liquid to obtain sodium p-nitrophenolate. According to the invention, the quaternary ammonium salt surfactant is added in the synthesis of sodium p-nitrophenolate, so that the reaction is milder, the occurrence of side reaction caused by black material formation due to too fast local reaction is prevented to a certain extent, and the yield and the purity are further improved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemical products, and in particular relates to a synthesis process of sodium p-nitrophenolate. Background technique [0002] Sodium p-nitrophenolate is an important fine chemical intermediate, which can be used as a raw material for the manufacture of pesticides parathion and methyl parathion. After acidification and reduction, p-aminophenol can be obtained, and the latter is a developer, medicine and dye The production process of sodium p-nitrophenolate is as follows: Add a sodium hydroxide solution with a certain volume concentration of 133-136g / L into the hydrolysis kettle, then add quantitatively molten p-nitrochlorobenzene, and fill it with 0.8kg of air / cm 2 After heating the temperature of the material to 157°C, the pressure in the kettle is 0.6Mpa, then stop heating, the exothermic hydrolysis reaction makes the temperature and pressure rise naturally to 168°C, 0.75Mpa, and cool...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/22C07D233/06B01F17/32B01F17/18C09K23/18C09K23/32
CPCC07C201/12C07D233/06C09K23/00C07C205/22
Inventor 陈斌陈永贵过学军黄中桂熊刚姚翔曹明晶
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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