Synthesizing method and device for o-nitrochlorobenzene

The technology of a nitrile benzyl chloride and a synthesis method, which is applied in the field of organic synthesis methods and devices thereof, can solve the problems of low cost, high cost, heavy pollution product purity, etc., and achieves reduction of suction filtration process, improvement of safety, and shortening of fractionation time. Effect

Inactive Publication Date: 2018-05-08
武穴市阳泰化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] In order to solve the problems of high cost, heavy pollution and low product purity in the traditional production process, the present invention provides an environmentally friendly synthesis method and device for o-cyano-cyanobenzyl chloride with short reaction time, high product purity and greatly reduced cost

Method used

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  • Synthesizing method and device for o-nitrochlorobenzene
  • Synthesizing method and device for o-nitrochlorobenzene
  • Synthesizing method and device for o-nitrochlorobenzene

Examples

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Embodiment 1

[0051] In the present embodiment, a kind of synthetic method of o-cyano benzyl chloride comprises the following steps:

[0052] In the first step, the o-methylbenzonitrile liquid is passed into the reactor 1 at a speed of 30 kg per hour, and the temperature in the reactor 1 is slowly raised to 125° C., the ultraviolet light source 35 in the reactor 1 is opened, and The speed of 10kg per hour is passed into chlorine in the reactor 1;

[0053] In the second step, when the feed rate of the o-methylbenzonitrile liquid in the reactor 1 reached 45% of the internal volume of the still, the feed of the o-tolunitrile liquid and chlorine gas was stopped, and after leaving standstill for 0.5 hour, then According to the feed speed of o-methyl benzonitrile liquid and chlorine in the first step, in reactor 1, pass into the o-methyl benzonitrile liquid and the chlorine of the first step, the o-methyl benzonitrile liquid and the first step After the introduction of chlorine gas is completed,...

Embodiment 2

[0072] In the present embodiment, in the present embodiment, a kind of synthetic method of o-cyano benzyl chloride comprises the following steps:

[0073] In the first step, the o-methylbenzonitrile liquid is passed into the reactor 1 at a speed of 30 kg per hour, and the temperature in the reactor 1 is slowly raised to 130° C., the ultraviolet light source 34 in the reactor 1 is opened, and The speed of 11kg per hour is passed into chlorine in reactor 1;

[0074] In the second step, when the feed rate of the o-methylbenzonitrile liquid in the reactor 1 reached 45% of the internal volume of the still, the feed of the o-tolunitrile liquid and chlorine gas was stopped, and after leaving standstill for 0.5 hour, then According to the feed speed of o-methyl benzonitrile liquid and chlorine in the first step, in reactor 1, pass into the o-methyl benzonitrile liquid and the chlorine of the first step, the o-methyl benzonitrile liquid and the first step After the introduction of chl...

Embodiment 3

[0092] In the present embodiment, in the present embodiment, a kind of synthetic method of o-cyano benzyl chloride comprises the following steps:

[0093] In the first step, the o-methylbenzonitrile liquid is passed into the reactor 1 at a speed of 30 kg per hour, and the temperature in the reactor 1 is slowly raised to 135° C., the ultraviolet light source in the reactor 1 is turned on, and every The speed of hour 12kg is passed into chlorine in reactor 1;

[0094] In the second step, when the feed rate of the o-methylbenzonitrile liquid in the reactor 1 reached 45% of the internal volume of the still, the feed of the o-tolunitrile liquid and chlorine gas was stopped, and after leaving standstill for 0.5 hour, then According to the feed speed of o-methyl benzonitrile liquid and chlorine in the first step, in reactor 1, pass into the o-methyl benzonitrile liquid and the chlorine of the first step, the o-methyl benzonitrile liquid and the first step After the introduction of c...

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Abstract

The invention relates to the field of organic synthesizing methods and devices thereof, in particular to a synthesizing method and a synthesizing device for o-nitrochlorobenzene. The synthesizing method comprises the following steps in sequence: performing photochlorination on a mixed liquid A, performing distilling and separating on a mixed liquid B, performing condensing and recycling on a mixedliquid C, performing suction filtration and separation on a mixed liquid D, performing centrifuge-dripping on coarse o-nitrochlorobenzene and drying o-nitrochlorobenzene powder; in addition, the device for implementing the synthesizing method comprises a reaction kettle for implementing the photochlorination, a distilling kettle, a receiving kettle and a finished product kettle which are used forperforming distilling and separating on the mixed liquid B, and a suction filtration trough, a centrifugal machine and a drying room which are used for crystallizing and separating the o-nitrochlorobenzene from the mixed liquid D; compared with the conventional synthesizing process, the synthesizing time consumption required by the synthesizing method is greatly reduced; the purity of the finished o-nitrochlorobenzene reaches 99 percent; meanwhile, the safety and the reliability of a synthesizing process are also improved; produced exhaust is also recycled; the synthesizing method and the synthesizing device have extremely good popularization and application prospect.

Description

technical field [0001] The invention relates to the field of an organic synthesis method and a device thereof, in particular to a method and a device for synthesizing o-cyanobenzyl chloride. Background technique [0002] O-cyanobenzyl chloride is a colorless to jade-colored needle-like crystal at room temperature. It is a monochlorobenzyl compound with a melting point and a boiling point of 59.5°C and 252-260°C, respectively. It is mainly used for the synthesis of diphenyl Ethylene fluorescent whitening agent, such as fluorescent whitening agent ER series, is an important industrial intermediate raw material. [0003] In the existing synthetic technology, o-cyanobenzyl chloride mainly utilizes o-toluonitrile to be synthesized under the conditions of passing chlorine and light, and its reaction route is: [0004] [0005] During this period, it needs to be processed by reaction kettle, distillation kettle, crystallization kettle, centrifuge and drying. [0006] Taking a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/30C07C253/34
CPCC07C253/30C07C253/34C07C255/50
Inventor 吴水保王碧江
Owner 武穴市阳泰化工股份有限公司
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