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A kind of preparation method of 1-chlorobutane

A technology of chlorobutane and hydrogen chloride, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of unfavorable industrialized production, long post-processing time, and high production costs, and achieves short post-processing time and cost. Low, low equipment requirements

Active Publication Date: 2016-03-30
LIANHE CHEM TECH (DEZHOU) CO LTD +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the existing 1-chlorobutane preparation method when there is no catalyst, the equipment used is complicated, and the production cost is high; There will be a large amount of metal ions in the wastewater in the process, and the environmental pollution is serious; when N-methylimidazole hydrochloride ionic liquid is used as the chlorination reagent, the post-treatment takes too long, which is not conducive to technical problems such as industrial production, and A preparation method of 1-chlorobutane is provided

Method used

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  • A kind of preparation method of 1-chlorobutane
  • A kind of preparation method of 1-chlorobutane

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Experimental program
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Effect test

Embodiment 1

[0031] After adding concentrated hydrochloric acid (33.5% by mass, 653.0 g, 6.0 mol) and dimethyl sulfoxide (0.31 g, 0.004 mol) into a four-neck round bottom flask, stir at 20-30°C for 30 min. Add n-butanol (149.0g, 2.0mol), slowly raise the temperature to 90°C-100°C, and distill while reacting. As the reaction time prolongs, fractions will slowly distill out gradually. After about 20hrs of heat preservation distillation and reaction, almost no If any fraction was further distilled, the reaction was considered to be complete. After the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 170.3 g of 1-chlorobutane was obtained, with a yield of 91.5% and a GC purity of 99.7%.

Embodiment 2

[0033]After implementing 1 reaction, finally get the reaction liquid raffinate 531.0g, continuously pass into HCl gas wherein, after passing through for a period of time, sampling detection, HCl content is 34.6%, stop passing into HCl gas, at this moment, after passing through HCl The total weight of the reaction liquid raffinate is: 654.1g. After adding 0.1 g of dimethyl sulfoxide, stir at 20-30°C for 30 min. Add n-butanol (149.0g, 2.0mol), slowly raise the temperature to 90-100°C, and distill while reacting. As the reaction time prolongs, fractions will gradually distill out. After about 20hrs of heat preservation distillation and reaction, almost no Fractions were further distilled, and the reaction was considered to be complete. After the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 172.5 g of 1-chlorobutane was obtained, with a yield of 92.7% and a GC purity of 99.6%.

Embodiment 3

[0035] Water (434.3g) was added into the four-neck round bottom flask, and HCl gas was continuously fed thereinto, so that the HCl content reached 45%, and the total weight of the reaction solution was 789.6g. Dimethylsulfoxide (0.78g, 0.01mol) was added and stirred at 15-20°C for 20min. Add n-butanol (149.0g, 2.0mol), slowly raise the temperature to 85-95°C, and distill while reacting. As the reaction time prolongs, fractions will gradually distill out. After 20hrs of heat-retaining distillation and reaction, there is almost no fraction After further distillation, the reaction was considered to be complete. After the obtained fractions were separated, the upper organic layer was 1-chlorobutane, and finally 174.7 g of 1-chlorobutane was obtained, with a yield of 93.5% and a GC purity of 99.6%.

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Abstract

The invention discloses a preparation method of 1-chlorobutane. The preparation method comprises the following steps: mixing a catalyst, a chlorination agent and water together, stirring, and then mixing the mixture with n-butyl alcohol to perform a chlorination reaction, thereby obtaining the 1-chlorobutane, wherein the catalyst is dimethyl sulfoxide; the chlorination agent is hydrogen chloride; the molar ratio of the chlorination agent to the n-butyl alcohol is 2.5:(1-5):1; the stirring is performed within a temperature range of 15-45 DEG C. According to the preparation method of the 1-chlorobutane, DMSO is taken as the catalyst and no any metal ion takes part in the whole process; the hydrogen chloride gas can be further introduced into the obtained final reaction liquid residue to increase the concentration of the HCl in the reaction liquid residue, so that the reaction liquid residue can be reused in next batch, few three wastes are generated and the environment is protected; meanwhile, the preparation method is simple in equipment, low in cost, convenient to operate, high in both yield and purity, and more suitable for industrial production. The reaction formula is as shown in the specification.

Description

technical field [0001] The invention 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 olefin polymerization catalyst - butyllithium, to prepare butyltin products through Grignard reaction, to prepare phenylbutazone in medicine, to prepare insecticide myclobutanil in pesticide, 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 follows: [0004] (1) According to the report of patent CN101475440, n-butanol an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/01C07C17/16
Inventor 银亮熊亮林行军奚奇何俊
Owner LIANHE CHEM TECH (DEZHOU) CO LTD
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