Method and equipment for preparing paranitrobenzoyl chloride

A technology of nitrobenzoyl chloride and p-nitrobenzoic acid, which is applied in the field of preparation of p-nitrobenzoyl chloride, can solve the problems of solvent residue, increased production cost and equipment investment, difficult handling of phosphorus oxychloride, etc., and achieves The production cycle is short, the distillation purification time is shortened, and the product yield is high.

Active Publication Date: 2015-03-11
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product yield of this process is high, but the reaction uses phosphorus trichloride chlorination agent, and the phosphorus oxychloride produced is difficult to handle, which increases the production cost and equipment investment, and the crystallization solvent is used in the process, so that the product is easy to have solvent residue

Method used

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  • Method and equipment for preparing paranitrobenzoyl chloride
  • Method and equipment for preparing paranitrobenzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Put 500Kg of p-nitrobenzoic acid and 1250Kg of thionyl chloride into the reaction kettle, add 2.5Kg of N,N-dimethylformamide, and carry out the reaction at 90°C until no gas comes out. Atmospheric distillation, then distillation under 600mmHg until no thionyl chloride flows out to obtain the p-nitrobenzoyl chloride crude product, and put into the overhead tank;

[0034] (2) Turn on the primary thin film evaporator, and heat up to 100°C; the secondary thin film evaporator, and heat up to 175°C;

[0035] (3) Adjust the vacuum of the first-stage thin film evaporator to be 720mmHg, start feeding, and uniformly add the crude product to the first-stage thin-film evaporator according to a certain sampling speed; the discharge enters the crude product storage tank, and the material in the crude product storage tank Enter into the secondary thin film evaporator through the magnetic pump;

[0036] (4) Adjust the vacuum degree of the secondary thin-film evaporator to be 730mm...

Embodiment 2

[0038] (1) Put 500Kg of p-nitrobenzoic acid and 1500Kg of thionyl chloride into the reactor, add 0.5Kg of N,N-dimethylformamide, and carry out the reaction at 90°C until no gas comes out. Atmospheric distillation, and then distilling under vacuum at 610mmHg until no thionyl chloride flows out, obtains the crude product of p-nitrobenzoyl chloride, and puts it into the overhead tank;

[0039] (2) Turn on the primary thin film evaporator, and heat up to 120°C; the secondary thin film evaporator, and heat up to 165°C;

[0040] (3) Adjust the vacuum of the first-stage thin film evaporator to 700mmHg, start feeding, and uniformly add the crude product to the first-stage thin-film evaporator according to a certain sampling speed; the discharge enters the crude product storage tank, and the material in the crude product storage tank Enter into the secondary thin film evaporator through the magnetic pump;

[0041] (4) Adjust the vacuum degree of the secondary thin-film evaporator to b...

Embodiment 3

[0043] (1) Put 500Kg of p-nitrobenzoic acid and 1750Kg of thionyl chloride into the reaction kettle, add 5Kg of N,N-dimethylformamide, and react at 90°C until no gas comes out. pressure distillation, and then distilled under 630mmHg until no thionyl chloride flows out to obtain the p-nitrobenzoyl chloride crude product, and put it into the overhead tank;

[0044] (2) Turn on the primary thin film evaporator, and heat up to 130°C; the secondary thin film evaporator, and heat up to 155°C;

[0045] (3) Adjust the vacuum degree of the first-level thin film evaporator to be 660mmHg, start feeding, and add the crude product to the first-level thin film evaporator evenly by a certain sampling speed; the discharge enters the crude product storage tank, and the crude product storage tank The material enters the secondary thin film evaporator through the magnetic pump;

[0046] (4) Adjust the vacuum degree of the secondary thin-film evaporator to be 750mmHg, start feeding, and the mate...

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Abstract

The invention belongs to the technical field of fine chemical engineering, and in particular relates to a method and equipment for preparing paranitrobenzoyl chloride. The method comprises the following steps: performing a refluxing reaction on nitrodracylic acid and thionyl chloride under the effect of a catalyst, distilling and recycling the thionyl chloride under the normal pressures and the reduced pressure respectively after the reaction so as to obtain a crude product of the paranitrobenzoyl chloride; allowing the crude product to enter into an one-stage film evaporator through a high-level tank to distil the residual thionyl chloride at a reduced pressure, and then distilling and refining a reactant by a two-stage film evaporator under the condition of high vacuum so as to obtain the paranitrobenzoyl chloride. In the method, the two stages of the film evaporators are adopted in the refining process, because the heat transfer area is large and the efficiency is high, the residual thionyl chloride and the residual catalyst in reaction liquid can be effectively removed, time for distilling and refining is shortened, side effects and impurities are prevented, and the method has the characteristics that the method is simple and practicable to operate, the production cycle is short, the product yield is high, and the impurity content is low; the production equipment disclosed by the invention has the advantages that the operation is convenient, and the work efficiency is substantially improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method and equipment of p-nitrobenzoyl chloride. Background technique [0002] p-Nitrobenzoyl chloride is an important intermediate in the synthesis of folic acid, procaine hydrochloride, N-p-aminobenzoyl-L-glutamic acid and other vitamin pharmaceutical products, and is also widely used in the production of pigments and color developers . Especially in recent years, with the rise of feed industry and the development of information industry, the consumption of p-nitrobenzoyl chloride is increasing. [0003] "Journal of Natural Sciences of Xiangtan University" at the end of September 1994, Volume 16, No. 3 "Synthesis of p-nitrobenzoyl chloride by melting crystallization method", using p-nitrobenzoic acid and phosphorus trichloride, using carbon tetrachloride as a solvent, Chlorine gas is passed into the reaction material, and the reaction temperat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/57C07C201/12
CPCY02P20/584
Inventor 薛居强张泰铭孙丰春张聪聪杨德耀宋国城张善民毕义霞谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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