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Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof

A technology for deodorizing distillate and oil, applied in chemical instruments and methods, preparation of steroids, organic chemistry, etc., to achieve considerable economic value, protect the environment, and reduce the discharge of waste residues.

Inactive Publication Date: 2009-12-23
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

None of the above patents involves the separation and extraction of natural phytosterols from the residual oil after molecular distillation of vegetable oil deodorization distillates

Method used

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  • Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof
  • Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof
  • Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 1Kg soybean deodorized distillate residue and 1000mL water into the reactor, heat to 100°C, stir for 60 minutes to mix the two evenly, then add 0.4Kg calcium oxide to the reactor, react at 100°C for 3 hours, add The hydrochloric acid was neutralized to pH=6, and the lower aqueous layer was separated and removed. Transfer the oil phase to a cold analysis kettle, then add 1000mL ethanol to the oil phase, heat to 70°C, stir until the oil phase is completely dissolved, then lower the temperature at a rate of 10°C / hour, and keep the stirring speed at 1.5 rpm during the cooling process When a large number of tiny grains are formed, heat and stir for 2 hours, and then continue to cool down at 4°C / hour. When the temperature reaches 15°C, stop stirring, keep the temperature at 15°C, and mature for 6 hours. Subsequently, the crystallization solution was transferred to a plate and frame filter press for pressure filtration, and the filter cake was washed with 1000 mL of ethano...

Embodiment 2

[0030] Add 1Kg of rapeseed oil deodorized distillate residue and 500mL of ethanol into the reactor, heat to 70°C, stir for 30 minutes to mix the two evenly, then add 3Kg of sodium hydroxide to the reactor, and react at 80°C for 2 hours , add sulfuric acid to neutralize to pH = 1, separate and remove the lower aqueous layer. Transfer the oil phase to a cold analysis kettle, then add 1000mL of petroleum ether to the oil phase, heat to 60°C, stir until the oil phase is completely dissolved, then lower the temperature at a rate of 8°C / hour, and keep the stirring speed at 1.5 rpm during the cooling process / min, when a large number of tiny crystal grains are formed, heat and stir for 1 hour, then continue to cool down at 2°C / hour, stop stirring when the temperature reaches 5°C, keep the temperature at 5°C, and mature for 12 hours. Then the crystallization solution was transferred to a plate and frame filter press for pressure filtration, and the filter cake was washed with 1000 mL ...

Embodiment 3

[0032]Add 1Kg of soybean oil deodorized distillate residue and 750mL of n-propanol into the reactor, heat to 90°C, stir for 30 minutes to mix the two evenly, then add 0.3Kg of potassium hydroxide to the reactor, and react at 97°C After 5 hours, sulfuric acid was added to neutralize to pH=5, and the lower aqueous layer was separated and removed. Transfer the oil phase to a cold analysis kettle, then add 2500mL of organic solvents listed in Table 1 to the oil phase, heat to 60°C, stir until the oil phase is completely dissolved, then cool down at a rate of 5°C / hour, and keep The stirring speed is 1.5 rpm. When a large number of tiny grains are formed, keep stirring for 1 hour, and then continue to cool down at 1°C / hour. When the temperature reaches 5°C, stop stirring, keep the temperature at 5°C, and mature for 24 hours. Subsequently, the crystallization solution was transferred to a plate and frame filter press for pressure filtration, and the filter cake was washed three times...

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Abstract

The invention relates to a catalytic decomposition and solvent crystallization technique for extracting and purifying natural phytosterol from oil deodorization distillate. The technique comprises the process as follows: vegetable oil and fat deodorization distillate residual oil and solvent are put into a reaction kettle to be heated for catalytic decomposition; after water layers are separated, oil phase is transferred into a cold separation tower and added with organic solvent for dynamic gradient cooling crystallization; after being processed by curing heat preservation and filtration, the crude product of phytosterol can be obtained; finally, the crude product is processed by secondary solvent crystallization, and the purified product of the phytosterol can be obtained. Phytosterol ester in the residual oil can be transformed into phytosterol by catalytic decomposition; as the dynamic gradient crystallization technique is adopted, the quality and the yield of the product can be improved. The phytosterol prepared by the technique has the purity being more than 90%, so as to meet the market demand. The yield of the phytosterol reaches to 5-40% of the raw material residual oil, and after the solvent of the filtrate of the separated phytosterol is recovered, residue can be taken as rust preventive oil. The technique is simple, convenient in operation, good in controllability, low in cost and easy in industrialization.

Description

technical field [0001] The invention relates to the field of biochemical industry, in particular to a catalytic decomposition and solvent crystallization purification process for extracting natural phytosterols from oil deodorization distillate residue. Background technique [0002] Phytosterols widely exist in plants and plant seeds, and are one of the components of cell membranes in plants. Phytosterol is a natural substance with important physiological value. It is non-toxic and has good emulsification and stability. Therefore, it is widely used in various fields such as medicine, food, daily chemicals, animal growth agents, chemicals, and textiles. related industries. Phytosterols contain sitosterol, campesterol, brassicasterol, stigmasterol and other components, which have strong anti-inflammatory and anti-inflammatory effects and are directly used as anti-inflammatory drugs. It has been proved clinically at home and abroad that natural phytosterols have important phy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00C07J75/00
Inventor 严峰李建新吴道庚杨昊鋆曹玉平蒋一鸣
Owner TIANJIN POLYTECHNIC UNIV
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