Preparation method of high purity butyl lactate

A technology of butyl lactate and high purity, applied in the field of preparation of high-purity butyl lactate, can solve the problems of long esterification reaction time, unfavorable industrialized production, complicated process, etc., shorten the esterification reaction time, and improve the conversion rate of lactic acid. , the effect of simplifying the refining operation

Active Publication Date: 2013-05-15
JIANGSU YIDA CHEM
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Problems solved by technology

[0004] Chinese patent CN102030644 discloses a preparation method of butyl lactate. This patent uses lactic acid and n-butanol as raw materials, and uses sulfuric acid-loaded activated clay as a catalyst. The disadvantages are: sulfuric acid is too acidic, and the post-treatment is complicated, causing much pollution.
Chinese patent CN1450046 discloses a high-yield, high-optical-purity L-butyl lactate synthesis method. This patent uses lactic acid and n-butanol as raw materials, and uses concentrated sulfuric acid as a catalyst. Aftertreatment, anhydrous sodium carbonate is used to neutralize sulfuric acid. Its disadvantages are: adopting traditional neutralization and water washing process, the discharge of waste water is large and the pollution is serious
Chinese patent CN101914021 discloses a two-step method for producing butyl lactate with high content and high optical purity. In this patent, lactic acid is used as raw material to synthesize lactide, and then refined lactide and n-butanol are used as raw materials to synthesize butyl lactate. Its disadvantages are: complex process, low yield, long esterification reaction time, unfavorable for industrial production

Method used

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Experimental program
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Effect test

Embodiment 1

[0012] Add 169 g of industrial lactic acid, 445 g of n-butanol, and 185 g of benzene into the flask. Add 2.50 g of self-made potassium bisulfate and ferric chloride composite catalyst. The esterification reaction is carried out in the esterification tower, the vacuum degree of the esterification reaction device system is 55kPa, the esterification reaction time is 3 hours, and the esterification reaction temperature is 110°C. Lactic acid conversion rate was 96%. The obtained reaction liquid was subjected to vacuum distillation operation. The vacuum degree of the distillation system is 10kPa, and the distillation temperature is 130°C. Perform rectification operation on the distilled cuts to separate high-purity butyl lactate with a purity of 99.9%.

Embodiment 2

[0014] 169 g of industrial lactic acid, 390 g of n-butanol, and 170 g of benzene were added to the flask. Add 2.35 g of self-made p-toluenesulfonic acid and sodium bisulfate composite catalyst. The esterification reaction is carried out in the esterification tower, the vacuum degree of the esterification reaction device system is 40kPa, the esterification reaction time is 2 hours, and the esterification reaction temperature is 120°C. Lactic acid conversion rate was 94%. The obtained reaction liquid was subjected to vacuum distillation operation. The vacuum degree of the distillation system is 10kPa, and the distillation temperature is 130°C. Perform rectification operation on the distilled cuts to separate high-purity butyl lactate with a purity of 99.9%.

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Abstract

The invention relates to a preparation method of high purity butyl lactate. The method is characterized by: taking industrial lactic acid and n-butyl alcohol as raw materials, and adopting benzene as a water-carrying agent, subjecting them to an esterification reaction in the presence of a catalyst, then carrying out vacuum distillation and refining, thus obtaining the high purity butyl lactate. Specifically, the catalyst is a composite catalyst of potassium hydrogen sulfate and ferric trichloride, or a composite catalyst of p-toluenesulfonic acid and sodium hydrogen sulfate. The method provided in the invention shortens the esterification reaction time, increases the yield of butyl lactate, simplifies refining operation, and is easy to realize industrialization.

Description

technical field [0001] The invention relates to a preparation method of high-purity butyl lactate. It belongs to the field of petrochemical industry. Background technique [0002] The chemical name of butyl lactate is alpha-hydroxypropionate butyl ester, which is a butyl ester derivative of lactic acid produced by the fermentation of carbohydrates similar to sugar and butanol. It is a colorless transparent liquid with a sweet taste. Cream aroma and milk aroma, easily soluble in most organic solvents such as ethanol, ether, acetone, esters, etc., partially hydrolyzed when miscible with water, non-toxic, good solubility, and completely biodegradable in nature. [0003] Butyl lactate is widely used in chemical, pharmaceutical, food and other industries. Solvent-grade butyl lactate is a high-quality green and environmentally friendly high-boiling solvent used in natural resins, synthetic resins, spices, paints, printing inks, dry cleaning fluids, and adhesives. Special specif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/68C07C67/08C07C67/54B01J27/128B01J31/26
Inventor 刘准祝义鹏曹惠庆张虎
Owner JIANGSU YIDA CHEM
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