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Method for continuously synthesizing chlorobutane in non-aqueous system

A technology of chlorobutane and system, which is applied in the field of continuous synthesis of chlorobutane, can solve the problems of low efficiency and high energy consumption, and achieve the effects of shortening the process flow, simple operation and short reaction time

Pending Publication Date: 2022-01-07
山东绿色海洋化工研究院有限公司 +1
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Problems solved by technology

[0003] A preparation method of 1-chlorobutane disclosed in Chinese patent CN104326863A uses dimethyl sulfoxide as a catalyst to catalyze the reaction of hydrogen chloride and n-butanol to generate 1-chlorobutane, the yield can reach 89.6~93.5%, and the purity can reach 99.5~99.7% %, the reaction time of this method needs 20 hours, low efficiency and high energy consumption
[0004] Chinese patent CN1440958 (CN1225440C) discloses the method that primary alcohol or cyclohexanol in acidic ionic liquid [Hmim]+X-(X=Cl, Br, I) is converted into halogenated hydrocarbon, with n-butanol and N-methylimidazole Hydrochloride ionic liquid reaction, in which N-methylimidazole hydrochloride is used as a solvent and provides chlorine element to participate in the chlorination reaction. This process is a batch process with a reaction time of 12 hours and low efficiency. Concentrated hydrochloric acid is needed after the reaction is completed. Regeneration of N-Methylimidazolium Hydrochloride Ionic Liquid

Method used

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  • Method for continuously synthesizing chlorobutane in non-aqueous system

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: the method for the continuous synthesis of chlorobutane in a kind of non-aqueous system

[0019] Include the following steps:

[0020] Add 10 kilograms of 1-butyl-3-methylimidazolium chloride salt at the bottom of the reactive distillation column 1 and pass it into the reboiler 6 for circulation, open the reboiler 6 to make the whole system of the reactive distillation column 1 warm up to 120 ± 2 ℃, and then pass 1-butyl-3-methylimidazolium chloride into the falling film evaporator 5 to raise the temperature to 110 ℃. Open the second circulating pump 7, and the ionic liquid enters the reactive distillation tower 1 in the form of spray from the top of the first tower section of the reactive distillation tower 1 after the falling film evaporator 5, and the flow rate of the spray is 210g / min, and then At the top of the first tower section, n-butanol was introduced at a flow rate of 74g / min, and hydrogen chloride gas was introduced at the bottom of the tower ...

Embodiment 2

[0023] Add 10 kg of 1-butyl-3-methylimidazolium chloride salt to the bottom of reactive distillation tower 1, the temperature in the entire system of reactive distillation tower 1 is raised to 90±2°C, the temperature of falling film evaporator 5 is raised to 100°C, other processes The conditions were the same as in Example 1, and reflux began to occur at the top of the tower after 30 minutes of feeding hydrogen chloride gas.

[0024] Example 2, take an instant sample (initial distillation) at the top of the tower after 30 minutes of feeding for analysis, the content of 1-chlorobutane is 95.56%, the content of n-butanol is 2.87%, n-butyl ether is 1.110%, and isomers are 0.082%. Others 0.378%; 1 hour and 45 minutes after the introduction, take an instant sample from the top of the tower for analysis, 1-chlorobutane content 87.13%, n-butanol content 11.18%, n-butyl ether 0.48%, isomers 0.047%, other 1.163 %; 10 hours after the introduction, take an instant sample from the top of ...

Embodiment 3

[0026] Add 10 kg of 1-butyl-3-methylimidazolium chloride salt to the bottom of reactive distillation tower 1, the temperature in the entire system of reactive distillation tower 1 is raised to 150±2°C, the temperature of falling film evaporator 5 is raised to 120°C, and the top of the tower The reflux temperature was controlled at 90±1° C., and the other process conditions were the same as in Example 1. The reflux began to appear at the top of the tower after 30 minutes of hydrogen chloride gas feeding.

[0027] Example 3, take an instant sample (initial distillation) at the top of the tower after 30 minutes for analysis, the content of 1-chlorobutane is 99.87%, the content of n-butanol is 0.049%, n-butyl ether is 0.0094%, and isomers are 0.0512%. Others 0.0204%; 1 hour and 45 minutes after the introduction, take an instant sample from the top of the tower for analysis, 1-chlorobutane content 98.74%, n-butanol content 0.23%, n-butyl ether 0.0113%, isomers 0.141%, other 0.8777 ...

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Abstract

The invention relates to a method for continuously synthesizing chlorobutane in a non-aqueous system. The method is characterized in that a non-aqueous system is composed of an ionic liquid 1-butyl-3-methylimidazolium chloride or 1-butylpyridine hydrochloride, n-butyl alcohol and hydrogen chloride, and the ionic liquid is both a solvent and a catalyst for a chlorination reaction; a chemical reaction for continuously synthesizing chlorobutane, n-butanol and hydrogen chloride and rectification of the reaction product 1-chlorobutane are synchronously and continuously carried out in a reaction rectification tower; and hydrogen chloride gas is introduced from the bottom of the reaction rectification tower, n-butanol and the ionic liquid are introduced from the middle of the reaction rectification tower, 1-chlorobutane is extracted from the top of the tower, and part of ionic liquid extracted from the bottom of the tower is subjected to moisture evaporating in a falling-film evaporator, and then returns to the system. According to the method, reaction and rectification are carried out at the same time, operation is simple, the reaction rate is high, almost instantaneous reaction occurs to generate 1-chlorobutane after gas-liquid two-phase contact, the ionic liquid can be regenerated after being simply dehydrated; the purity of 1-chlorobutane is greater than or equal to 99.5%, and the product yield is 90.3-98.2% in terms of n-butanol.

Description

technical field [0001] The invention relates to a method for continuously synthesizing chlorobutane in a non-aqueous system, belonging to the technical field of organic synthesis. Background technique [0002] 1-Chlorobutane, also known as n-butyl chloride and chlorobutane, is an important monovalent halogenated alkane, which can be used as solvent, organic synthesis intermediate and catalyst in the fields of oil, rubber and resin. There are many raw materials for synthesizing 1-chlorobutane. In industrial production, cheap n-butanol and hydrogen chloride gas or concentrated hydrochloric acid are mainly used as raw materials to synthesize 1-chlorobutane. The synthesis method has several disclosed in the following patents: [0003] A preparation method of 1-chlorobutane disclosed in Chinese patent CN104326863A uses dimethyl sulfoxide as a catalyst to catalyze the reaction of hydrogen chloride and n-butanol to generate 1-chlorobutane, the yield can reach 89.6~93.5%, and the pu...

Claims

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Application Information

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IPC IPC(8): C07C17/16C07C17/383C07C19/01
CPCC07C17/16C07C17/383C07C19/01Y02P20/10Y02P20/54
Inventor 王德强类成存杨树仁杨睿君崔淑娜张文静黄志杰王启元赵家林郐丽马淑敏王美芹丁国军黄伟
Owner 山东绿色海洋化工研究院有限公司
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