Summary of the invention
The present invention has overcome the deficiencies in the prior art, a kind of method of extracting natural Coenzyme Q10 99.0 with the palm slag has been proposed, method raw material provided by the invention is cheap and easy to get, flow process is simple, operational path is shorter, energy consumption is lower, in the Coenzyme Q10 99.0 oil that obtains, Coenzyme Q10 99.0 content is higher, and the multiple beneficial such as rich vitamin A, vitamin-E material can be directly as foodstuff additive.
Technical solution of the present invention is: a kind of method of extracting natural Coenzyme Q10 99.0 with the palm slag, described method is at first dry with the palm slag, then take supercritical co as extraction agent, described dry palm slag is extracted, then after the CO 2 fluid that obtains being carried out decompression separation, can obtain being rich in the oil of Coenzyme Q10 99.0, described method comprises following concrete steps:
1) obtain dry palm slag after the palm slag is dried, its water content is 10%~20%;
2) take supercritical co as extraction agent, described dry palm slag is extracted, obtain CO 2 fluid;
3) described CO 2 fluid is carried out decompression separation twice, obtain being rich in the oil of Coenzyme Q10 99.0.
Preferably, described step 2) in, the temperature of described extraction is 35 ℃~60 ℃.
Preferably, described step 2) in, the pressure of described extraction is 15MPa~35MPa.
Preferably, described step 3) comprising:
A) described CO 2 fluid is carried out first step decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0;
B) described CO 2 fluid through first step decompression separation is carried out second stage decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0.
Preferably, the pressure of described first step decompression separation is 5MPa~7MPa.
Preferably, the temperature of described first step decompression separation is 35 ℃~50 ℃.
Preferably, the pressure of described second stage decompression separation is 2MPa~8MPa.
Preferably, the temperature of described second stage decompression separation is 30 ℃~40 ℃.
Compared with prior art, the present invention is at first dry with the palm slag, then take supercritical co as extraction agent, described dry palm slag is extracted, and after then the CO 2 fluid that obtains being carried out decompression separation, can obtain being rich in the oil of Coenzyme Q10 99.0.The present invention extracts the oil that is rich in Coenzyme Q10 99.0 take supercritical co as extraction agent, extraction efficiency is high, and raw material is cheap and easy to get, obtain oily Coenzyme Q10 99.0 content high, productive rate is high, functional component is abundant, active high, steady quality.Experiment shows, adopts in the oil that is rich in Coenzyme Q10 99.0 that method provided by the invention obtains, and the content of Coenzyme Q10 99.0 is greater than 30%, and contains abundant vitamin-E and vitamin A etc.
Simultaneously, method provided by the invention need not to carry out complicated pre-treatment operation, the palm slag is dry, can directly extract after being crushed to 20 orders left and right, extract the complete rear oil that decompression separation can obtain being rich in Coenzyme Q10 99.0 that directly carries out, need not complicated aftertreatment technology, flow process is simple, operational path is short, energy consumption is low.In addition, the present invention does not with an organic solvent extract, and the Coenzyme Q10 99.0 product that obtains can not be subject to the heavy metal contamination of organic solvent residual.
Embodiment
The invention provides a kind of method of extracting natural Coenzyme Q10 99.0 with the palm slag, comprise the following steps:
A) the palm slag is carried out drying, obtain the raw material of the broken conduct extraction of looking over so as to check of dry palm ground-slag;
B) the palm slag to described drying extracts take supercritical co as extraction agent, obtains being rich in the CO 2 fluid of Coenzyme Q10 99.0 oil;
C) described CO 2 fluid is carried out decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0.
The present invention carries out the extraction of natural Coenzyme Q10 99.0 take palm slag (skin slag and pomace) as raw material take supercritical co as extraction agent, extraction efficiency is high, and the oily active constituent content that is rich in Coenzyme Q10 99.0 that obtains is high, productive rate is high, steady quality.
The present invention extracts the oil that is rich in Coenzyme Q10 99.0 take the palm slag as raw material.Gained palm slag is carried out drying, obtain dry palm slag.
After obtaining dry palm slag, through pulverizing and sieving, take supercritical co as extraction agent, described dry palm slag is extracted.All higher than its critical temperature Tc (31.1 ℃) with during emergent pressure Pc (7.39MPa), be called supercritical co when the temperature T of carbonic acid gas and pressure P.Supercritical co has gas property and liquid property concurrently, has stronger dissolving power, can improve product purity during as extraction agent, increases productive rate.
At first the present invention is condensed into liquid with carbon dioxide take carbon dioxide as extraction agent, after then making carbonic acid gas be in supercritical state by the control temperature and pressure, described dry palm slag is extracted.According to the present invention, the temperature when extracting is preferably 35 ℃~60 ℃, and more preferably 40 ℃~55 ℃, most preferably be 40 ℃~50 ℃, the pressure when extracting is preferably 15MPa~35MPa, more preferably 18MPa~20MPa.
In extraction process, the oil that is rich in Coenzyme Q10 99.0 in dry palm slag is dissolved in supercritical co, separates with cell debris etc., obtains CO 2 fluid.After obtaining CO 2 fluid, it is carried out the oil that decompression separation can obtain being rich in Coenzyme Q10 99.0.
Described decompression separation process preferably includes following steps:
Described CO 2 fluid is carried out first step decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0;
Described CO 2 fluid through first step decompression separation is carried out second stage decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0.
At first described CO 2 fluid is carried out first step decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0.The pressure of described first step decompression separation is preferably 5MPa~12MPa, more preferably 5MPa~7MPa; The temperature of described first step decompression separation is preferably 35 ℃~50 ℃, more preferably 40 ℃~45 ℃.
Through still containing the oil that part is rich in Coenzyme Q10 99.0 in the CO 2 fluid after first step decompression separation, it is carried out second stage decompression separation, obtain being rich in the oil of Coenzyme Q10 99.0.The pressure of described second stage decompression separation is preferably 2MPa~8MPa, more preferably 2.5MPa~4MPa; The temperature of described second stage decompression separation is preferably 30 ℃~40 ℃, more preferably 33 ℃~38 ℃.Through after two-stage decompression separation, the oily major part that is rich in Coenzyme Q10 99.0 is separated.
Below in conjunction with accompanying drawing, the present invention is described with the method that the palm slag extracts natural Coenzyme Q10 99.0.
Referring to accompanying drawing, at first dry palm slag is placed in extractor 5, with extractor 5 sealings;
Open gas-holder 1, carbonic acid gas is converted into liquid through condenser 2, becomes supercritical co after heating via high-pressure pump 3 pressurizations and preheater 4, enters in extractor 5 wherein dry palm slag is extracted;
Extract complete after, be dissolved with the CO 2 fluid that is rich in Coenzyme Q10 99.0 oil and enter the first separating tank 6, make carbonic acid gas and be rich in the separating of oil of Coenzyme Q10 99.0 by step-down, the oil that is rich in Coenzyme Q10 99.0 is discharged by the blow-off valve 8 on the first separating tank 6;
CO 2 fluid through the first separating tank 6 enters the second separating tank 7, again make carbonic acid gas after step-down and be rich in the separating of oil of Coenzyme Q10 99.0, the oil that is rich in Coenzyme Q10 99.0 is discharged by the blow-off valve 8 on the second separating tank 7, and carbonic acid gas is recyclable to be reused to condenser 2.
After obtaining being rich in the oil of Coenzyme Q10 99.0, the described oil that is rich in Coenzyme Q10 99.0 is detected, its Coenzyme Q10 99.0 content is greater than 30%.
The present invention extracts the oil that is rich in Coenzyme Q10 99.0 take the palm slag as raw material, productive rate is high, Coenzyme Q10 99.0 content and active high, steady quality.Simultaneously, method raw material provided by the invention is cheap and easy to get and need not to carry out complicated pre-treatment operation through simply pulverizing and sieving, can directly extract after drying, extract the complete rear oil that decompression separation can obtain being rich in Coenzyme Q10 99.0 that directly carries out, need not complicated aftertreatment technology, flow process is simple, operational path is short, energy consumption is low.In addition, the present invention does not with an organic solvent extract, and the Coenzyme Q10 99.0 product that obtains can not be subject to the heavy metal contamination of organic solvent residual.
In order to further illustrate the present invention, below in conjunction with embodiment, the method with the natural Coenzyme Q10 99.0 of palm slag extraction provided by the invention is described in detail.
Embodiment 1
The palm slag is dry, obtain dry palm slag; It was pulverized 20 mesh sieves
The palm slag that adds the described drying and crushing of 1000g in the extractor 5, the sealing extractor; 5 open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 30MPa, the condition of 50 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 10MPa, the condition of 45 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 40 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 2h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 150.9g is rich in Coenzyme Q10 99.0, percentage extraction is 15.09%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 30.20%.
Embodiment 2
The palm slag is dry, obtain dry palm slag;
The palm slag that adds the described drying of 1000g in the extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 25MPa, the condition of 50 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 9MPa, the condition of 50 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 30 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 2h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 141.88g is rich in Coenzyme Q10 99.0, percentage extraction is 14.188%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 30.80%.
Embodiment 3
The palm slag is dry, obtain dry palm slag;
Add the described dry palm slag of 1000g in extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 18MPa, the condition of 45 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 8MPa, the condition of 45 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 30 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 2h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 121.3g is rich in Coenzyme Q10 99.0, percentage extraction is 12.13%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 30.52%.
Embodiment 4
The palm slag is dry, obtain dry palm slag;
Add the described dry palm slag of 1000g in extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 20MPa, the condition of 35 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 8MPa, the condition of 35 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 30 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 2h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 129.6g is rich in Coenzyme Q10 99.0, percentage extraction is 12.96%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 30.99%.
Embodiment 5
The palm slag is dry, obtain dry palm slag;
The palm slag that adds the described drying of 1000g in the extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 15MPa, the condition of 60 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 8MPa, the condition of 50 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 40 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 2h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 112.2g is rich in Coenzyme Q10 99.0, percentage extraction is 11.22%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 31.08%.
Embodiment 6
The palm slag is dry, obtain dry palm slag;
The palm slag that adds the described drying of 5000g in the extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 20MPa, the condition of 50 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 8MPa, the condition of 45 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 40 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 6h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 134.5g is rich in Coenzyme Q10 99.0, percentage extraction is 13.45%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 31.12%.
Embodiment 7
The palm slag is dry, obtain dry palm slag;
Add the described dry palm slag of 5000g in extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 18MPa, the condition of 50 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 8MPa, the condition of 45 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 3MPa, the condition of 40 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 6h, obtain altogether being rich in the oil of Coenzyme Q10 99.0 from the first separating tank 6 and the second separating tank 7, percentage extraction is 12.66%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 30.88%.
Embodiment 8
The palm slag is dry, obtain dry palm slag;
Add the described dry palm slag of 5000g in extractor 5, sealing extractor 5; Open gas-holder 1, keeping the flow of carbonic acid gas is 480L/h, carbonic acid gas enters described extractor 5 after condenser 2, high-pressure pump 3 and preheater 4, extract under 15MPa, the condition of 60 ℃, CO 2 fluid after extraction enters the first separator, carry out the first step and separate under 10MPa, the condition of 50 ℃, obtain first part of oil that is rich in Coenzyme Q10 99.0; CO 2 fluid after separating through the first step continues to enter the second separator, carries out the second stage and separate under 5MPa, the condition of 40 ℃, obtains second part of oil that is rich in Coenzyme Q10 99.0.
After dynamic extraction 6h, obtain altogether from the first separating tank 6 and the second separating tank 7 oil that 253g is rich in Coenzyme Q10 99.0, percentage extraction is 11.94%, and in the described oil that is rich in Coenzyme Q10 99.0, the content of Coenzyme Q10 99.0 is 31.05%.
The above is only the preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.