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Method for preparing high-purity ricinus oil according to chromatographic separation

A castor oil, high-purity technology, applied in the direction of oil/fat refining, fat production, etc., can solve the problem of no high-purity castor oil

Inactive Publication Date: 2016-04-20
NANJING WELL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the preparation of high-purity castor oil (ricinoleic acid in castor oil fatty acid > 99%, ricinoleic acid triglyceride content > 98%) by chromatography separation and purification in various literature patents

Method used

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  • Method for preparing high-purity ricinus oil according to chromatographic separation
  • Method for preparing high-purity ricinus oil according to chromatographic separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation of embodiment 1 high-purity castor oil

[0026] Under normal temperature and pressure, 1 kg of coarse-pore 100-200 mesh silica gel, n-hexane, ethyl acetate volume ratio of 6:1 eluent was stirred into a homogenate and then added to the chromatography column. After the silica gel was solidified, the buffer was added Quartz sand, 100g crude castor oil was dissolved in 300ml eluent, stirred evenly, added to the chromatography column, and eluted for 30min; the eluent with a volume ratio of n-hexane and ethyl acetate of 4:1 was eluted for 90min; The column pressure is 0.5MPa, and the eluent with a volume ratio of n-hexane and ethyl acetate of 1:1 is eluted for 30 minutes, analyzed by TLC, and the iodine cylinder is used for color development, and high-purity castor oil is collected. Half of the solution volume is heated at 80°C. Wash twice with salt water, dry the oil layer with anhydrous sodium sulfate, filter, and distill under reduced pressure to obtain 66 ...

Embodiment 2

[0030] The preparation of embodiment 2 high-purity castor oil

[0031] Under normal temperature and pressure, 1 kg of coarse-pore 100-200 mesh silica gel and n-hexane, ethyl acetate, acetic acid volume ratio of 6:1:0.1 eluent was stirred into a homogenate and added to the chromatography column, and the silica gel was solidified Finally, add buffering agent quartz sand, dissolve 100g crude product castor oil in 300ml eluent, stir evenly, add in the chromatographic column, and elute for 30min; the volume ratio of n-hexane, ethyl acetate and acetic acid is 7:3 : 0.1 eluent elution 90min; pressure 0.5MPa, n-hexane, ethyl acetate and acetic acid volume ratio of 1:1:0.1 eluent elution 30min, TLC analysis, iodine cylinder color development, collection of high purity castor oil, half of the volume of the solution was washed twice with hot brine at 80°C, the oil layer was dried with anhydrous sodium sulfate, filtered, and distilled under reduced pressure to obtain 53 g of castor oil, w...

Embodiment 3

[0032] The preparation of embodiment 3 high-purity castor oil

[0033] 1 kg of coarse-pore 100-200 mesh silica gel and V petroleum ether: V ethyl acetate = 4:1 eluent were stirred into a homogenate and then added to the chromatography column. After the silica gel was solidified, the buffer quartz sand was added, and 100g Crude castor oil was dissolved in 300ml eluent, stirred evenly and added to the chromatographic column, chromatographic separation, TLC analysis, iodine cylinder color development, high-purity castor oil was collected, vacuum distillation, and the obtained oil was added to 3g of Clay clay and 3g of gac, decolouring under 90 ℃ of temperature vacuum degree-0.098MPa 2 hours, the high-purity castor oil after distillation and decolouring is press-filtered under 0.5MPa with the press filter that macromolecule precision microporous membrane is housed, thereby Obtain 59g of high-purity castor oil, the yield is 59%. After testing, the castor oil fatty acid contains ric...

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Abstract

The invention provides a method for preparing high-purity ricinus oil according to chromatographic separation. The method comprises the following steps: (1) selecting a proper stationary phase, and filling a glass column of an appropriate inside diameter with the stationary phase uniformly to obtain a chromatographic column; (2) preparing eluents of different polarity gradients, and diluting a ricinus oil crude product with the eluents according to a certain proportion; (3) loading according to a dry or wet method; (4) conducting gradient segmented elution on a sample with the eluents of different polarities at an ordinary temperature, wherein in each gradient, Rf is 0.1 to 0.9, the Delta Rf of separated components is larger than 0.1, the pressure is normal pressure to 1 MPa, the elution flow velocity is 0.1 to 8 cm / min, and the ricinus oil crude product interacts with the stationary phase via chromatography, so as to realize separation; (5) analyzing each obtained component, and carrying out collection, concentration, decolorization and pressure filtration to obtain high-purity ricinus oil, wherein the fatty acid in the fat of the ricinus oil contains 99% or higher of ricinoleyl alcohol, and the fat of the ricinus oil contains 98% or higher of ricinoleyl alcohol triglyceride.

Description

technical field [0001] The invention relates to chromatographic separation to prepare high-purity castor oil, that is, a preparation method for chromatographic separation to prepare high-purity castor oil alkyd and high-purity castor oil alkyd triglyceride. technical background [0002] Castor oil is one of the top ten oil crops and one of the four major inedible oil crops in the world. It is mainly produced in Brazil, India and the former Soviet Union, and is planted in all provinces of my country. Castor oil is obtained by pressing and refining castor oil. It is the only commercial oil mainly containing hydroxy acids. Castor oil is a very important chemical raw material, which can be directly used as a pharmaceutical raw material, and can also be used as a synthetic resin, paint, paint, soap, ink, plasticizer, emulsifier, lubricant, engine oil, brake fluid, Antifungal agents, food additives, seasonings, flavors and other industries, widely used in textile, chemical, light...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11B3/00C11B3/10
Inventor 刘清峰王保成朱兵徐璠峰吴仰波
Owner NANJING WELL CHEM
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