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A kind of esterification-ultrahigh pressure crystallization separation method of vegetable oil distillate

A technology for separation of vegetable oil distillate and crystallization, which is applied in the field of separation technology, can solve the problems of long separation time, low resource utilization rate, low product yield, etc., and achieves the effects of significant synergy, small loss, and reduced production cost.

Active Publication Date: 2015-09-16
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are many methods for separating the functional components of vegetable oil distillates, such as saponification, urea encapsulation, solvent extraction, etc., but in order to remove free fatty acids, it is often necessary to decompose neutral oil; The resource utilization rate is not high, and the separation time is long and the product yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add absolute ethanol (distillate mass: ethanol mass = 1:1) and concentrated sulfuric acid (1-2% of the distillate mass) to the soybean oil distillate, and heat at 80°C for 1 hour to esterify the free fatty acid. Filter the esterification liquid, inject the filtrate into the urea-95% ethanol (distillate mass: urea mass: 95% ethanol mass = 1:2:5) solution, dissolve evenly, pour it into a soft package, put it into an ultra-high pressure container after sealing, and apply 350MPa, hold pressure for 1 hour; release pressure, take out the solution containing crystals, filter, concentrate to remove ethanol, wash to remove urea, concentrate and dry again to obtain polyunsaturated fatty acid ethyl ester, VE, squalene, phytosterol and neutral oil VE recovery rate ≥ 90%; phytosterol recovery rate ≥ 60%; squalene recovery rate ≥ 70%; neutral oil recovery rate ≥ 90%; ethyl linoleate recovery rate ≥ 80%. Rate ≥ 60%.

Embodiment 2

[0023] Add absolute ethanol (distillate mass: ethanol mass = 1:1) and concentrated sulfuric acid (1-2% of the distillate mass) to the soybean oil distillate, and heat at 80°C for 1 hour to esterify the free fatty acid. Filter the esterification liquid, inject the filtrate into the urea-95% ethanol (distillate mass: urea mass: 95% ethanol mass = 1:2:5) solution, dissolve evenly, pour it into a soft package, put it into an ultra-high pressure container after sealing, and apply 500MPa, hold the pressure for 0.5 hours; release the pressure, take out the solution containing crystals, filter, concentrate to remove ethanol, wash to remove urea, concentrate and dry again to obtain polyunsaturated fatty acid ethyl ester, VE, squalene, phytosterol and neutral oil VE recovery rate ≥ 90%; phytosterol recovery rate ≥ 60%; squalene recovery rate ≥ 70%; neutral oil recovery rate ≥ 90%; ethyl linoleate recovery rate ≥ 80%. Rate ≥ 60%.

Embodiment 3

[0025] Add absolute ethanol (distillate mass: ethanol mass = 1:1) and concentrated sulfuric acid (1-2% of the distillate mass) to the distillate of Camellia oleifera seed oil, heat and react at 80°C for 1 hour to make free fatty acid ethyl esterification . Filter the esterification liquid, inject the filtrate into the urea-95% ethanol (distillate mass: urea mass: 95% ethanol mass = 1:2:5) solution, dissolve evenly, pour it into a soft package, put it into an ultra-high pressure container after sealing, and apply 350MPa, keep the pressure for 1 hour, release the pressure, take out the crystal-containing solution, and filter; add urea-ethanol solution to the filtrate as before, repeat the ultra-high pressure crystallization once, and filter; the filter residue contains a large amount of ethyl oleate (can be extracted and used separately) The filtrate is concentrated to remove ethanol, washed with water to remove urea, and then concentrated and dried to obtain products containing...

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Abstract

An esterification-ultrahigh pressure crystallization separation method for a distillate of vegetable oil takes the distillate of vegetable oil as a raw material, comprises the various unit processes of esterifying, crystalizing, separating, desolventizing, washing and drying, and is characterized in that: in the esterifying process, concentrated sulfuric acid is taken as a catalyst, and absolute ethyl alcohol and free fatty acid are subject to esterification reaction at the temperature of 80 DEG C for 1 hour; in the crystalizing process, urea and 95% ethyl alcohol are added into an esterifying solution, the mixture is stirred to be dissolved, injected into a soft packaging bag, pumped and sealed, and then put into an ultrahigh pressure container to be processed at the pressure of 100-600MPa for 0.5-1h, then the pressure is released, the bag is unpacked, and the operations of separating, desolventizing, washing and drying are conducted to obtain a product mainly containing unsaturated fatty acid ethyl ester, VE, squalene, phytosterol and neutral oil. According to the method, the recovery rate of VE is equal to or larger than 90%, the recovery rate of phytosterol is equal to or larger than 60%, the recovery rate of squalene is equal to or larger than 70%, the recovery rate of neutral oil is equal to or larger than 90%, and the recovery rate of ethyl linoleate is equal to or larger than 80%.

Description

1. Technical field [0001] The invention relates to a separation process, in particular to an esterification-ultrahigh pressure crystallization separation method of vegetable oil distillates. 2. Background technology [0002] Vegetable oil vacuum deodorization distillate (hereinafter referred to as vegetable oil distillate) contains a large amount of VE (vitamin E), squalene, phytosterols, polyunsaturated fatty acids and other functional components, a large amount of neutral oil (grease) and saturated fatty acids, monounsaturated fatty acids, etc. Unsaturated fatty acids; in addition, it also contains impurities such as saturated hydrocarbons, odorous substances, and pigments. [0003] In order to separate functional components from vegetable oil distillates, free fatty acids, pigments, saturated hydrocarbons, odorous substances and other impurities must be removed. [0004] There are many methods for separating the functional components of vegetable oil distillates, such as...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/52C07C67/60C07C69/587C11C3/00C11C3/04C11B3/00C11B3/02C07J9/00C07C11/21C07C7/148C07C7/14
Inventor 潘见孙艳辉徐金凤惠爱玲金日生琚裕杰赵斌张星
Owner 潘见
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