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Preparation method of 1-chlorobutane

A technology of chlorobutane and n-butanol, which is applied in the field of preparation of 1-chlorobutane, can solve the problems of high equipment requirements, many by-products, and complex processes, and achieve the effects of good safety, less three wastes, and simple processes

Active Publication Date: 2021-04-27
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to provide a preparation method of 1-chlorobutane, which solves the problems of complex process, high equipment requirements, large pollution and many by-products in the existing synthesis process, and has the advantages of simple and easy operation, continuous production, The advantages of environmental protection and pollution-free, high product yield and high product purity are more suitable for industrial production

Method used

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  • Preparation method of 1-chlorobutane
  • Preparation method of 1-chlorobutane
  • Preparation method of 1-chlorobutane

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 200ml of 2,3,5,6-tetramethyldioxane, 20ml of purified water, and 200ml of n-butanol (2.19mol) into a 1000ml three-necked flask equipped with a stirrer and a thermometer, and stir to raise the temperature to 105°C , feed 199.8g (5.48mol) of hydrogen chloride gas, and distill while reacting. As the reaction time prolongs, fractions will slowly distill out gradually. After completing the heat preservation distillation and reacting for 2 hours, almost no further fractions will distill out, and the reaction is over. , after the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 195.4g (2.11mol) of 1-chlorobutane was obtained, the molar yield was 96.3%, and the GC purity was 99.83%. The chromatographic results are shown in figure 1 and Table 1. The 1-chlorobutane standard product is calibrated by GC, and the obtained product is 1-chlorobutane with a retention time of 3.968'; at the same time, n-butanol and dibutyl ether are calibrat...

Embodiment 2

[0046] Add 300ml of 2,3,5,6-tetramethyldioxane, 20ml of purified water, and 200ml of n-butanol (2.19mol) into a 1000ml three-necked flask equipped with a stirrer and a thermometer, and stir to raise the temperature to 115°C , feed 196.4g (5.38mol) of hydrogen chloride gas, and distill while reacting. As the reaction time prolongs, fractions will slowly distill out gradually. After completing the insulation distillation and reacting for 2 hours, almost no further fractions will distill out, and the reaction is over. After the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 195.9 g (2.12 mol) of 1-chlorobutane was obtained, with a molar yield of 96.6% and a GC purity of 99.79%.

Embodiment 3

[0048]Add 100ml of 2,3,5,6-tetramethyldioxane, 20ml of purified water, and 200ml of n-butanol (2.19mol) into a 1000ml three-necked flask equipped with a stirrer and a thermometer, and stir to raise the temperature to 85°C , feed 239.8g (6.57mol) of hydrogen chloride gas, and distill while reacting. As the reaction time prolongs, fractions will slowly distill out. After the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 194.6 g (2.11 mol) of 1-chlorobutane was obtained, with a molar yield of 96.0% and a GC purity of 99.87%.

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Abstract

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a preparation method of 1-chlorobutane. A reaction solvent, water and n-butyl alcohol are mixed, and a chlorination reagent is added for reaction to obtain 1-chlorobutane, wherein the reaction solvent is 2, 3, 5, 6-tetramethyl dioxane. A one-pot method is adopted, and the method is simple, good in safety, easy to implement, low in equipment requirement and capable of realizing continuous production. The problem of heavy pollution of the traditional metal catalyst is avoided, three wastes are few, and the method is environment-friendly. 2, 3, 5, 6-tetramethyl dioxane is used as a reaction solvent and a catalyst, so that the generation of byproducts such as butene, dibutyl ether and polymer resin can be effectively avoided, the yield and the product quality are improved, the molar yield of the product is 96% or above, and the gas phase purity is 99.7% or above.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 1-chlorobutane. Background technique [0002] 1-Chlorobutane is an important fine chemical product, which can be used in oils and fats, rubber, natural resin solvents, pharmaceutical intermediates, co-catalysts, etc. At present, it is mainly used to prepare butyllithium, an olefin polymerization catalyst, to prepare butyltin products through Grignard reaction, to prepare phenylbutazone in medicine, to prepare the insecticide myclobutanil in pesticides, and to produce polyether. Used as a solvent. At present, more than 99% of products are required in the market, and the purity of 1-chlorobutane used for synthesizing n-butyllithium is required to be ≥99.5%. [0003] The prior art mainly uses n-butanol and hydrochloric acid or hydrogen chloride gas as raw materials to synthesize 1-chlorobutane, and the main synthetic methods are as follow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C19/01B01J31/02
CPCC07C17/16B01J31/0201C07C19/01
Inventor 邱化齐李璞李剑
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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