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Method used for preparing lauric acid from litsea cubeba fruit kernel oil

A technology of lauric acid and nucleolus oil, which is applied in the preparation of oxygenated compounds, the preparation of organic compounds, the preparation of carboxylate/lactone, etc. problems such as high pressure, to achieve the effect of solvent recycling, simplifying operation and reducing investment costs

Inactive Publication Date: 2018-06-26
黄石市禾呈林业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the purity of lauric acid in mixed fatty acids is very high, lauric acid can be separated by pressing, so it must be rectified to obtain sufficiently pure lauric acid, so that the rectification process takes a long time, consumes a lot of energy, and costs high. At the same time, rectification High equipment investment costs and low production efficiency
When the purity of lauric acid in the mixed fatty acid is not high, it needs to be distilled again; when there are impurities close to the melting and boiling point of lauric acid, it is difficult to obtain lauric acid with higher purity by combining rectification and pressing
In addition, the squeezer also needs to apply a lot of pressure, which consumes a lot of energy.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: Take 15 kg of crushed and sieved Litsea cubeba processing residue, add 210 L of petroleum ether (boiling range of 60 to 90 ° C), reflux at 80 ° C for 2 h, cool, filter, and the filtrate is rotary evaporated to obtain nucleolus Oil, dried to constant weight at 60 ℃, weighed

[0014] Obtained 3.9 kg kernel oil.

[0015] Take 500 mL Litsea cubeba kernel oil, preheat to 70 °C under stirring, add 10 mL of 95%-98% concentrated sulfuric acid, stir for 5 min, add 25 mL of water, continue stirring for 30 min, stop stirring and keep warm for 30 min Cool to room temperature, pour out the upper layer of oil, wash with water until neutral to obtain 480 mL of oil, and the lower layer is a pitch-like substance.

[0016] Take 400 mL of acid-refined kernel oil, preheat it to 75 °C under stirring, add 200 mL of 1 mol / L NaOH solution, stir evenly, and measure the pH to 11; then add 50 mL of 35% dilute Sulfuric acid, stir evenly, boil for 5 minutes, stop stirring, keep warm fo...

Embodiment 2

[0019] Example 2: Take 30 kg of crushed and sieved Litsea cubeba processing residue, add 420 L of petroleum ether (boiling range of 60 to 90 ° C), reflux at 80 ° C for 2 h, cool, filter, and the filtrate is rotary evaporated to obtain nucleolus oil, dried at 60°C to constant weight, and 8.1 kg of kernel oil was weighed.

[0020] Take 1000 mL Litsea cubeba kernel oil, preheat to 70°C under stirring, add 20 mL of 95%-98% concentrated sulfuric acid, stir for 5 min, then add 50 mL of water, continue stirring for 30 min, stop stirring and keep warm for 30 min Cool to room temperature, pour out the upper layer of oil, wash with water until neutral to obtain 990 mL of oil, and the lower layer is a pitch-like substance.

[0021] Take 800 mL of acid-refined kernel oil, preheat it to 75°C under stirring, add 400 mL of 1mol / L NaOH solution, stir evenly, and measure the pH to 11; then add 100 mL of dilute sulfuric acid with a volume ratio of 35%, After stirring evenly, boil for 5 minutes...

Embodiment 3

[0024] Example 3: Take 45 kg crushed and sieved Litsea cubeba processing residue, add 620 L of petroleum ether (60-90 °C boiling range), reflux at 80 °C for 2 h, cool, filter, and the filtrate is rotary evaporated to obtain nucleolus oil, dried at 60°C to constant weight, and weighed to obtain 12.2kg of kernel oil.

[0025] Take 1500 mL Litsea cubeba kernel oil, preheat to 70 °C under stirring, add 30 mL of 95%-98% concentrated sulfuric acid, stir for 5 min, add 75 mL of water, continue stirring for 30 min, stop stirring for 30 min and then cool to room temperature, pour out

[0026] The oily layer was washed with water until neutral to obtain 1480 mL of oil, and the lower layer was bitumen-like substance.

[0027] Take 1200 mL of acid-refined kernel oil, preheat to 75°C under stirring, add 600 mL of 1 mol / L NaOH solution, stir evenly, and measure the pH to 11; then add 150 mL of 35% dilute Sulfuric acid, stir evenly, boil for 5 minutes, stop stirring, keep warm for 20 minut...

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Abstract

The invention relates to a method used for preparing lauric acid from litsea cubeba fruit kernel oil. The method comprises following steps successively: acid refining, hydrolysis, rectification, refrigeration solvent crystallization, pumping filtration, and drying; in the step of rectification, simple rectification is adopted, and the purity of obtained lauric acid is increased to 70%; in the stepof refrigeration solvent crystallization, a mixed solvent prepared from n-hexane or cyclohexane and ethanol at a volume ratio of 4-4.5:1 is adopted; under normal pressure, the preferable temperatureof refrigeration solvent crystallization ranges from -15 DEG C to -20 DEG C. In the method, routine rectification is replaced by simple rectification, rectification operation is simplified, speed is fast, energy consumption is low, investment cost is low, production benefit is increased, refrigeration solvent crystallization operation is simple, the solvent can be recycled, the method is economical, and is friendly to the environment, and the purity of obtained lauric acid is 98.0% or higher.

Description

technical field [0001] The invention relates to a process for extracting and purifying lauric acid from litsea cubeba kernel oil. Background technique [0002] Litsea cubeba is one of the unique spice resources in southern my country. Litsea cubeba oil is rich in citral, which is a raw material for the synthesis of ionone, ironone, etc. Litsea cubeba oil is often extracted by steam distillation in industry; Nucleolus oil can also be extracted from the Litsea cubeba residue of litsea cubeba oil, which is rich in natural oils and can be used to extract fatty acids, among which lauric acid is the most important one. Lauric acid is a saturated straight-chain dodecanoic acid, which can be used in the production of alkyd resins, wetting agents, detergents, insecticides, surfactants, food additives, etc. It is an important raw material for chemical, coating and other industries. [0003] In order to extract lauric acid from Litsea cubeba kernel oil, Cheng Sixi[Study on Extracting V...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/09C07C27/02C07C51/42C07C51/43C07C51/44C07C53/126
CPCC07C51/09C07C51/42C07C51/43C07C51/44C07C53/126
Inventor 程妍
Owner 黄石市禾呈林业有限公司
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