CN107903997A - A kind of method for preparing grease again using the dry shrimp slag of krill degreasing as raw material - Google Patents

Abstract

The invention discloses a kind of method for preparing grease again using the dry shrimp slag of krill degreasing as raw material, include the following steps：1) it is the dry shrimp sizing of krill degreasing is thin, obtain shrimp ground-slag；2) ethanol that mass concentration is 90 96% is added into shrimp ground-slag, high pressure homogenizer is injected after mixing, in 90 120MPa, high-pressure homogeneous 30 60min；3) homogeneous liquid is filtered, boils off ethanol, obtain grease.In liquid after homogeneous, shrimp ground-slag further crushes, reduce the diffusion path length between the intracellular grease of shrimp ground-slag and ethanol extractant, and when being extracted using 90 96% ethanol, most grease in dry shrimp slag can quickly be dissolved, intracellular grease concentration is improved, both comprehensive functions so that be easier to extract the remaining grease in shrimp slag cell.

Description

A method for preparing oil from Antarctic krill defatted dried shrimp dregs as raw material

technical field

The invention relates to a method for preparing oil by taking defatted dried Antarctic krill dregs as raw materials, and belongs to the fields of food, chemistry and medicine.

Background technique

Antarctic krill is a huge amount of biological resources living in the Antarctic Ocean (about 500-500000000 tons, different estimation methods are different). Antarctic krill is rich in oil, and the oil content varies with seasons, ages, genders, richness of food, environment and other factors. Oil is rich in unsaturated fatty acids (such as EPA, DHA, DPA, etc.), astaxanthin and its lipids, phospholipids, vitamin E and other nutrients. At present, Antarctic krill oil is a high value-added product widely sold in the world. In the past, Antarctic krill oil products were mainly produced in Canada, Japan, Norway, and the United States. After 2009, many manufacturers in my country have begun to produce Antarctic krill oil that meets international standards.

The method of extracting shrimp oil from krill is mainly to disperse krill in an organic solvent or a mixture of different organic solvents for extraction, and the protein content in the remaining krill dried shrimp dregs has reached more than 74%. Compared with the undefatted krill, the percentages of ash and amino acids in dried shrimp dregs have increased to a certain extent. After degreasing, most of the oil (shrimp oil) in the krill has been extracted, and the remaining oil remains in the shrimp dregs, which is difficult to extract using traditional shrimp oil extraction methods. Therefore, it is necessary to study and explore a new lipid extraction method suitable for dried shrimp dregs after degreasing.

Contents of the invention

Aiming at the technical problems existing in the above-mentioned prior art, the purpose of the present invention is to provide a method for preparing oil with the Antarctic krill defatted dried shrimp dregs as raw material, which can further extract the small amount of oil remaining in the defatted dried shrimp dregs , improve the oil yield of Antarctic krill, and improve the competitiveness of shrimp oil products.

In order to solve the above technical problems, the technical solution of the present invention is:

A method for preparing fat from Antarctic krill degreased dried shrimp dregs as raw material, comprising the following steps:

1) Grinding defatted dried Antarctic krill shrimp dregs to obtain shrimp dregs powder;

2) Add ethanol with a mass concentration of 90-96% to the shrimp dregs powder, mix well and inject into a high-pressure homogenizer, at 90-120MPa, high-pressure homogenize for 30-60min;

3) Filter the homogeneous liquid, evaporate ethanol to obtain oil.

The high-pressure homogenizer makes the mixed suspension of shrimp dregs powder and ethanol flow through the high-pressure homogeneous chamber at high speed under high pressure, and the material is subjected to mechanical forces such as high-speed shearing, high-frequency oscillation, cavitation and convective impact. The corresponding thermal effect makes the structure of the shrimp dregs powder change, and finally achieves a homogeneous effect. In the liquid after homogenization, ethanol can easily penetrate to the positions that are difficult to penetrate before the homogenization of the shrimp dregs powder, and then can extract the oil in the dead corner of penetration.

And, find through the test, in the liquid after the homogenization, the shrimp dregs powder is broken further, has reduced the diffusion path length between the fat in the shrimp dregs powder and the ethanol extractant, when adopting 90-96% ethanol to extract, can Quickly dissolve most of the oil in the dried shrimp residue, and the combined effect of the two makes it easier to extract the residual oil in the shrimp residue. Compared with the traditional organic solvent extraction method, the oil extraction efficiency can be greatly improved.

Preferably, in step 1), an agate ball mill is used to grind the Antarctic krill defatted dried shrimp dregs.

Further preferably, the volume of the agate balls housed in the agate ball mill jar is 30%-40% of the volume of the agate ball mill jar.

More preferably, the agate balls include large agate balls, medium agate balls and small agate balls, and the weight ratio of the large agate balls, medium agate balls and small agate balls is 2.5-3.5:10-12:5-7. The ratio of large, medium and small agate balls determines the unit impact area, impact force, number of impacts, and crushing speed of agate balls and shrimp residue particles, which is conducive to the simultaneous crushing of different sizes of particles and the turning of materials in different directions, so that the materials Evenly pulverized, when the material is uniformly pulverized, it is more conducive to improving the extraction rate of oil in the degreased dried shrimp dregs.

Further preferably, when using an agate ball mill to grind the Antarctic krill defatted dried shrimp residue, the revolution speed is 300-400rpm, the rotation speed is 400-800rpm, and the ball milling time is 1-2h.

When using an agate ball mill for grinding, the Antarctic krill defatted dried shrimp dregs can be ground to a finer fineness, which is convenient for the subsequent homogeneous extraction process. Moreover, ball milling by this method will not pollute the Antarctic krill degreased dried shrimp dregs, thus ensuring the quality of oil.

Further preferably, the particle size of the shrimp residue powder after ball milling is 110 mesh.

Preferably, in step 2), the quality of ethanol added is 10-20 times, preferably 15-20 times, that of the quality of shrimp dregs powder. To ensure that the oil in the shrimp dregs powder is better extracted.

Preferably, in step 2), the ethanol is ethanol with a mass concentration of 95%.

Preferably, in step 2), the flow rate of high pressure homogenization is 120-150ml/min, preferably 130-150ml/min, more preferably 130-140ml/min. When this flow rate is used, it is easier to homogenize the mixed suspension of defatted shrimp dregs powder and ethanol, and the homogenization effect is better. If the flow rate is too large or too small, the oil extraction rate in degreasing dried shrimp dregs will be affected.

Preferably, in step 3), the filtrate is rotated to remove the solvent at 68-72° C. to obtain oil.

The beneficial effects of the present invention are:

The high-pressure homogenizer makes the mixed suspension of shrimp dregs powder and ethanol flow through the high-pressure homogeneous chamber at high speed under high pressure, and the material is subjected to mechanical forces such as high-speed shearing, high-frequency oscillation, cavitation and convective impact. The corresponding thermal effect makes the structure of the shrimp dregs powder change, and finally achieves a homogeneous effect. In the homogenized liquid, ethanol can easily penetrate into the positions where the shrimp dregs powder is difficult to penetrate, and then the oil in the dead corner of penetration can be extracted.

In the homogenized liquid, the shrimp dregs powder is broken, which reduces the diffusion path length between the shrimp dregs powder oil and the ethanol extractant. The pressure release facilitates the rapid release of the solvent and the extracted oil at the same time. Moreover, when 90-96% ethanol is used for extraction, most of the oil in the dried shrimp dregs can be quickly dissolved. These combined effects can more easily extract the residual oil in the shrimp dregs.

Compared with the traditional organic solvent extraction method, the high-pressure homogenization of the suspension can greatly improve the extraction efficiency of oil.

Detailed ways

It should be pointed out that the following detailed description is exemplary and intended to provide further explanation to the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.

It should be noted that the terminology used here is only for describing specific implementations, and is not intended to limit the exemplary implementations according to the present application. As used herein, unless the context clearly dictates otherwise, the singular is intended to include the plural, and it should also be understood that when the terms "comprising" and/or "comprising" are used in this specification, they mean There are features, steps, operations, means, components and/or combinations thereof.

Embodiment one

Put 4 pieces of 150g Antarctic krill defatted dried shrimp dregs into 4 500ml agate ball mill jars of the ball mill, then add 23g of large agate balls, 83g of medium agate balls, and 45g of small agate balls in the jars. The rotation speed of the public adjustment is 350rpm, the self-rotation speed is 600rpm, and the ball milling time is 1.5h. Pour out the powder and sieve out the agate balls to get finely ground shrimp residue powder.

Take 10g of finely ground shrimp dregs powder, add 150ml of 95% ethanol to it, mix well and inject into a high-pressure homogenizer, at a working pressure of 100MPa, flow rate of 130ml/min, high-pressure homogenization for 45 minutes, pour out the feed liquid after homogenization .

The homogeneous feed liquid was filtered, and the filtrate was rotatively evaporated at 70° C. to remove the solvent to obtain 0.66 g of oil, with an oil yield of 6.6%.

Embodiment two

Put 4 pieces of 150g Antarctic krill defatted dried shrimp dregs into 4 500ml agate ball mill jars of the ball mill, then add 23g of large agate balls, 83g of medium agate balls, and 45g of small agate balls in the jars. The rotating speed of the public adjustment is 300rpm, the self-rotating speed is 800rpm, and the ball milling time is 2h. Pour out the powder and sieve out the agate balls to get finely ground shrimp residue powder.

Take 10g of finely ground shrimp dregs powder, add 100ml 95% ethanol to it, mix well and pour it into a high-pressure homogenizer. At a working pressure of 120MPa, a flow rate of 120ml/min, high-pressure homogenization for 60 minutes, pour out the feed liquid after homogenization .

The homogeneous liquid was filtered, and the filtrate was rotatively evaporated at 68° C. to remove the solvent to obtain 0.64 g of oil, with an oil yield of 6.4%.

Embodiment Three

Put 4 pieces of 150g Antarctic krill defatted dried shrimp dregs into 4 500ml agate ball mill jars of the ball mill, then add 23g of large agate balls, 83g of medium agate balls, and 45g of small agate balls in the jars. The rotation speed of the public adjustment is 400rpm, the self-rotation speed is 400rpm, and the ball milling time is 1h. Pour out the powder and sieve out the agate balls to get finely ground shrimp residue powder.

Take 10g of finely ground shrimp dregs powder, add 200ml of 95% ethanol to it, mix well and inject into a high-pressure homogenizer, at a working pressure of 90MPa, a flow rate of 150ml/min, high-pressure homogenization for 30 minutes, pour out the feed liquid after homogenization .

The homogeneous liquid was filtered, and the solvent was removed by rotary evaporation at 72° C. to obtain 0.68 g of oil, with an oil yield of 6.8%.

Comparative example one

The difference from Example 1 is: without high-pressure homogenization, 150ml of 95% ethanol is added to 10g of finely ground shrimp dregs powder, and directly extracted at 50°C for 45min to obtain 0.05g of oil and oil yield of 0.5%. It can be seen that if only 95% ethanol is used without high-pressure homogenization, it is difficult to achieve a good oil extraction effect.

Comparative example two

The difference from Example 1 is: without high-pressure homogenization, 150ml of 85% ethanol was added to 10g of finely ground shrimp dregs powder, and directly extracted at 50°C for 45min to obtain 0.05g of oil and oil yield of 0.5%.

Comparative example three

The difference with embodiment one is: the volume of the ethanol that adds in the shrimp dregs powder is 75ml, and other parameters are all identical with embodiment one, obtains grease 0.25g, obtains oil rate 2.5%.

The volume of the ethanol that adds in the shrimp dregs powder is 250ml, and other parameters are all identical with embodiment one, obtains oil 0.43g, obtains oil rate 4.3% (probably because too much ethanol has reduced the circulation in the shrimp dregs powder high-pressure homogenization Opportunity, but increased the time of the shrimp dregs powder in the circulating feed liquid tank to make part of the shrimp dregs powder precipitate from ethanol).

It can be seen that too large or too small amount of ethanol as the extraction solvent will affect the extraction efficiency of oil.

Comparative example four

The difference from Example 1 is: the organic extractant added to the shrimp dregs powder is acetone, and other parameters are the same as in Example 1 to obtain 0.13g of oil and 1.3% oil yield.

It can be seen that the change of extraction solvent can greatly change the oil extraction rate of degreased dried shrimp dregs.

Comparative example five

test 1

Add 8000ml of ethanol to 1kg of non-defatted Antarctic krill shrimp powder, stir and extract for 45 minutes, filter to obtain the filtrate, repeat the extraction of shrimp dregs for 2 times, combine the filtrate for 3 times and remove the solvent by rotary evaporation to obtain 160g of oil, and the yield of oil is 16.0 %.

test 2

The obtained defatted shrimp dregs filtered by test 1 are dried, and 4 150g dried shrimp dregs are put into 4 500ml agate ball mill jars of the ball mill, and then 23g of large agate balls, 83g of medium agate balls and 45g of small agate balls are added to the jar. The rotation speed of the public adjustment is 350rpm, the self-rotation speed is 600rpm, and the ball milling time is 1.5h. Pour out the powder and sieve out the agate balls to get finely ground defatted shrimp dregs powder.

Take 10g of finely ground defatted shrimp dregs powder, add 150ml of 95% ethanol to it, mix well and inject into a high-pressure homogenizer, at a working pressure of 100MPa, flow rate of 130ml/min, high-pressure homogenization for 45 minutes, pour out the material after homogenization liquid.

The homogeneous feed liquid was filtered, and the filtrate was rotatively evaporated at 70° C. to remove the solvent to obtain 0.65 g of oil, with an oil yield of 6.5%.

Test 3

Put 4 150g non-defatted dried Antarctic krill powder into 4 500ml agate ball mill jars of the ball mill, then add 23g of large agate balls, 83g of medium agate balls and 45g of small agate balls in the jars. The rotation speed of the public adjustment is 350rpm, the self-rotation speed is 600rpm, and the ball milling time is 1.5h. Pour out the powder, and sieve out the agate balls to get ground non-defatted shrimp powder.

Take 10g of ground non-defatted shrimp powder, add 150ml of 95% ethanol to it, mix well and pour it into a high-pressure homogenizer, at a working pressure of 100MPa, a flow rate of 130ml/min, high-pressure homogenization for 45 minutes, and pour out the material after homogenization liquid.

The homogeneous feed liquid was filtered, and the filtrate was rotatively evaporated at 70° C. to remove the solvent to obtain 1.63 g of oil, with an oil yield of 16.3%.

From the three experiments in Comparative Example 5, it can be seen that there is basically no difference in the oil obtained from the direct extraction of non-defatted Antarctic krill dried shrimp powder and the high-pressure homogeneous extraction after ball milling, and the shrimp powder with high oil content is difficult to crush into finer particles. It is easy to block when homogenizing and sinks quickly from the homogenizing solvent, and the ball milling and homogenization are poor. The degreased Antarctic krill dregs contain less oil, are crispy and easy to crush after drying, and are not clogged and difficult to settle when homogenized. Good results of ball milling and homogenization have been achieved. The method of the present invention is only suitable for the re-extraction of the remaining oil of defatted Antarctic krill residue.

The above descriptions are only preferred embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, there may be various modifications and changes in the present application. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of this application shall be included within the protection scope of this application.

Claims (10)

1. A kind of 1. method for preparing grease again using the dry shrimp slag of krill degreasing as raw material, it is characterised in that：Include the following steps：

   1) it is the dry shrimp sizing of krill degreasing is thin, obtain shrimp ground-slag；

   2) ethanol that mass concentration is 90-96% is added into shrimp ground-slag, injects high pressure homogenizer after mixing, in 90-120MPa, High-pressure homogeneous 30-60min；

   3) homogeneous liquid is filtered, boils off ethanol, obtain grease.
2. 2. according to the method described in claim 1, it is characterized in that：In step 1), krill is taken off using agate jar The dry shrimp slag of fat carries out levigate.
3. 3. according to the method described in claim 2, it is characterized in that：The volume for the agate ball being equipped with agate jar is agate The 30%-40% of ball milling tank volume.
4. 4. according to the method described in claim 3, it is characterized in that：The agate ball include big agate ball, middle agate ball and Small agate ball, the weight ratio of big agate ball, middle agate ball and small agate ball is 2.5-3.5:10-12:5-7.
5. 5. according to the method described in claim 4, it is characterized in that：Using agate jar to the dry shrimp slag of krill degreasing into When row is levigate, revolution rotating speed is 300-400rpm, and rotation rotating speed is 400-800rpm, Ball-milling Time 1-2h.
6. 6. according to the method described in claim 1, it is characterized in that：The granularity of shrimp ground-slag after ball milling is 110 mesh.
7. 7. according to the method described in claim 1, it is characterized in that：In step 2), the addition quality of ethanol is shrimp ground-slag quality 10-20 times, be preferably 15-20 times.
8. 8. according to the method described in claim 1, it is characterized in that：In step 2), the ethanol is that mass concentration is 95% Ethanol.
9. 9. according to the method described in claim 1, it is characterized in that：In step 2), high-pressure homogeneous flow is 120-150ml/ Min, is preferably 130-150ml/min, more preferably 130-140ml/min.
10. 10. according to the method described in claim 1, it is characterized in that：In step 3), filtrate is rotated under the conditions of 68-72 DEG C Evaporation of solvent, obtains grease.