Method for synthesizing high-purity butyl lactate

A technology of butyl lactate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of carboxylate, etc., can solve the problems of complicated preparation process, unsuitable for large-scale production, etc., and achieves simple operation and low cost. , the effect of low price

Inactive Publication Date: 2018-04-24
湖北华恒达化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The process of preparing high-purity butyl lactate reported in the literature needs to catalyze polycondensation of lactic acid into oligomers, and then depolymerize to obtain crude lactide, which is refined, and then refluxed with

Method used

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  • Method for synthesizing high-purity butyl lactate
  • Method for synthesizing high-purity butyl lactate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 200mL of water and 180.2g (2mol) of lactic acid into a 1000mL three-neck flask, stir, add dropwise an aqueous solution prepared by 84g (2.1mol) of sodium hydroxide at 20°C, and control the temperature of natural reaction not to exceed 90°C. After the addition is complete, continue Stir for 0.5 hours, distill under reduced pressure to remove water to dryness, cool down to 20°C, add 301.5 g (2.2 mol) of n-bromobutane dropwise, keep the reaction for 10 hours, add 600 mL of water to wash twice, and rectify the organic layer to obtain the product 282 grams, the gas chromatography content is 99.6%, and the molar yield is 96.5% based on lactic acid.

Embodiment 2

[0021] Add 200mL and 180.2g (2mol) of lactic acid into a 1000mL three-necked flask, stir, add dropwise an aqueous solution prepared by 138.3g (1mol) of potassium carbonate at 20°C, control the temperature of natural reaction not to exceed 90°C, and continue stirring for 1 hour after the dropwise addition is completed , distilled under reduced pressure to remove water to dryness, lowered the temperature to 20°C, added 274.1 g (2 mol) of n-bromobutane dropwise, raised the temperature to 40°C and kept the temperature for 8 hours, added 600mL water to wash twice, and rectified the organic layer to obtain the product 285.1 grams, the gas chromatography content is 99.5%, and the molar yield is 97.5% based on lactic acid.

Embodiment 3

[0023] Add 200mL and 180.2g (2mol) of lactic acid into a 1000mL three-necked flask, stir, add dropwise an aqueous solution prepared by 220.2g (2.2mol) of potassium bicarbonate at 20°C, and control the temperature of natural reaction not to exceed 90°C. After the addition is complete, continue stirring After 2 hours, remove water by distillation under reduced pressure to dryness, cool down to 20°C, add 274.1 g (2 mol) of brominated n-butane dropwise, raise the temperature to 60°C and keep the reaction for 5 hours, cool down to below 50°C, add 600mL water to wash twice, The organic layer was rectified to obtain 284.5 grams of the product, with a gas chromatographic content of 99.2%, and a molar yield of 97.3% based on lactic acid.

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Abstract

Provided is a method for synthesizing high-purity butyl lactate, and relates to the technical field of organic chemical synthesis. The method comprises the steps of: adopting lactic acid as a raw material, performing a reaction between the lactic acid and alkaline inorganic matter at a ratio in water to obtain lactate, performing distillation to remove water, performing a reaction between the lactate and n-butyl halide, and performing washing and rectification to obtain the high-purity butyl lactate, wherein the molar ratio of the lactic acid, alkaline inorganic matter and n-butyl halide is (1:0.5:1)-(1:1.1:1.5), the alkaline inorganic matter which is used for preparing the lactate includes one or a combination of more selected from sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium hydroxide and potassium hydroxide, and the n-butyl halide is one or a combination of more selected from n-butyl chloride and n-butyl bromide. The method has the advantages of low-cost raw materials, less equipment investment, mild reaction conditions and simple operation, and since water is adopted as a reaction solvent, the method is environmentally friendly and has low cost; the product can be purified easily, the purity can reach 99% or above, the yield can reach 95% or above, and therefore the method has a high economic value.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing high-purity butyl lactate. Background technique [0002] Butyl lactate is used as a solvent for the production of amine-based and nitro-based paints, as well as spices, synthetic resins, adhesives, etc. It is a relatively valuable intermediate for medicine and pesticides. The molecular structure is as follows: [0003] [0004] With the increasing demand for butyl lactate in food flavors and the increasing demand for high-purity lactic acid in synthetic medicine and pesticides, the market size of high-purity butyl lactate is expanding rapidly. [0005] At present, most of the domestic mainstream butyl lactate production methods use lactic acid and n-butanol to undergo esterification, and the products produced are all low-content products. [0006] The process of preparing high-purity butyl lactate reported in the literature needs t...

Claims

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Application Information

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IPC IPC(8): C07C67/11C07C69/68
CPCC07C51/412C07C67/11C07C59/08C07C69/68
Inventor 郭锐张伟略
Owner 湖北华恒达化工有限公司
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