Preparation method of 1 chlorobutane

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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.

1 chlorobutane is a kind of important fine chemical product, can be used for grease, rubber, natural resin solvent, medicine intermediate, promotor etc.At present mainly for the preparation of olefin polymerization catalysis-butyllithium, prepare butyl tin series products by grignard reaction, pharmaceutically for the preparation of Phenylbutazone, for the preparation of sterilant nitrile bacterium azoles on agricultural chemicals, use as solvent on polyethers is produced.And the product of existing market demand more than 99%, wherein for the synthesis of 1 chlorobutane purity requirement >=99.5% of n-Butyl Lithium.

In sum, in the preparation method of existing 1 chlorobutane, when using without catalyst system, the equipment of use is complicated, and equipment investment cost is high, is unfavorable for suitability for industrialized production; As use ZnCl 2and FeCl 3during catalyst system, heavy metal ions in wastewater content is higher, and environmental pollution is serious; When using N-methylimidazolium chloride ionic liquid, although can higher yields be obtained, but aftertreatment is consuming time more of a specified duration, production cycle is long, and production efficiency is low, is unfavorable for suitability for industrialized production, and, when reclaiming N-methylimidazolium chloride ionic liquid, energy consumption is higher, and meanwhile, whether the N-methylimidazolium chloride ionic liquid of recovery is applied mechanically higher yields can be kept not clear and definite.Therefore, this area needs a kind of preparation method of new 1 chlorobutane badly, has solved above-mentioned technical barrier.
Technical problem to be solved by this invention is in the preparation method in order to overcome existing 1 chlorobutane when catalyst-free exists, and the equipment of use is complicated, and production cost is high; When there being catalyzer to exist, generally use metal catalyst, have a large amount of metal ions in the waste water in last handling process, environmental pollution is serious; When adopting N-methylimidazolium chloride ionic liquid as chlorination reagent, aftertreatment is consuming time long, is unfavorable for the technical barriers such as suitability for industrialized production, and provides a kind of preparation method of 1 chlorobutane.The preparation method of present method, uses DMSO as catalyzer, participates in whole technological process without any metal ion; Gained end reaction liquid raffinate, can pass into hydrogen chloride gas again, and improve the concentration of HCl in reaction solution raffinate, and then apply mechanically in next batch, the three wastes are few, environmentally friendly; Meanwhile, preparation method's equipment of the present invention is simple, and cost is low, operates easy, and yield is in about 90%, GC purity more than 99.5%, and yield and purity are all higher, are more suitable for suitability for industrialized production.

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