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Preparation of chloro-cyclohexane under nitrogen protection

A technology for chlorocyclohexane and a preparation process is applied in the new technological field of safely preparing chlorocyclohexane, can solve problems such as increasing unsafe factors, and achieve the effects of preventing serial chlorination reactions and ensuring selectivity

Active Publication Date: 2009-02-18
SHANDONG YANGGU HUATAI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the inlets of cyclohexane and chlorine are in the reaction zone, the reaction starts before the materials are evenly mixed. Due to the high concentration of chlorine in the local area, there are still disadvantages of a series of chlorination reactions.
In addition, there are safety problems in the photochlorination of cyclohexane. If the reactor is coupled with the rectification tower, the temperature of the tower can reach 140-150 ° C, which increases the unsafe factor.

Method used

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  • Preparation of chloro-cyclohexane under nitrogen protection
  • Preparation of chloro-cyclohexane under nitrogen protection

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Embodiment Construction

[0015] The present invention is described in detail below in conjunction with embodiment.

[0016] Continuously feed cyclohexane from the bottom port of the reactor at a rate of 320-340 L / h, open the steam valve to raise the temperature of the reactor to 50-60°C. Mix chlorine gas and nitrogen gas at a volume ratio of 1: (0.5 ~ 1) and then continuously feed it from the side port at the bottom of the reactor. Adjust the flow valve so that the feed rate of chlorine gas is 70 ~ 80 kg / h. After the chlorine gas is diluted with nitrogen, it is fully mixed with cyclohexane in the mixing zone at the lower part of the reactor, and reaches the reaction zone (upper part of the reactor) equipped with an initiating light source, and reacts rapidly under the initiating light to generate chlorocyclohexane alkyl. The fed nitrogen plays an important protective role in the system safety response. The generated chlorocyclohexane overflows from the overflow pipe in time and continuously enters t...

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Abstract

The invention relates to a preparation method of chlorocyclohexane under the protection of nitrogen; the method is characterized in that the mixture of nitrogen and chlorine continuously is filled from the side opening of the lower part of a reactor, and cyclohexane is filled from the lower port of the reactor; the chlorine is pre-dispersed by the nitrogen, and then evenly mixed with the cyclohexane in the mixing area of the reactor, and enters into the reacting area of the reactor and reacts rapidly under the priming of the green ray to produce chlorocyclohexane which flows out of a overflow pipe, thereby improving the selectivity and the yield of the chlorocyclohexane. The nitrogen is continuously filled, so the reactor can be always in the state of nitrogen filling, which effectively prevents explosion accident.

Description

technical field [0001] The invention belongs to a synthesis process of organic chemical products, in particular to a new process for safely preparing chlorocyclohexane. Background technique [0002] Chlorocyclohexane is a basic raw material for organic synthesis and an important fine chemical product. It is mainly used in intermediates of rubber anti-scorch agent CTP, pharmaceutical dihemidylated hydrochloride, pesticide tricyclic tin and other products; it can also be used in polyurethane foaming catalyst N, N-dimethylcyclohexylamine, rust inhibitor, etc. synthesis. [0003] Among the many preparation methods of chlorocyclohexane, the cyclohexane photochlorination method overcomes the shortcomings of the cyclohexanol hydrogen chloride substitution method, cyclohexane chlorine replacement method, and cyclohexene hydrogen chloride addition method, because of its low reaction temperature , The reaction speed is fast, and the use of light source as the initiator avoids cataly...

Claims

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Application Information

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IPC IPC(8): C07C23/10C07C17/10
Inventor 王文博杜孟成孙庆刚郑崇纳王兴军许思俊师利龙马亚敏魏秋景
Owner SHANDONG YANGGU HUATAI CHEM
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