CN111500365A - Coconut oil catalytic crystal growing and fractionation method - Google Patents
Coconut oil catalytic crystal growing and fractionation method Download PDFInfo
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- CN111500365A CN111500365A CN202010244396.XA CN202010244396A CN111500365A CN 111500365 A CN111500365 A CN 111500365A CN 202010244396 A CN202010244396 A CN 202010244396A CN 111500365 A CN111500365 A CN 111500365A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0083—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils with addition of auxiliary substances, e.g. cristallisation promotors, filter aids, melting point depressors
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Abstract
The invention discloses a coconut oil catalytic crystal growing and fractionation method, which relates to the technical field of vegetable oil processing and comprises heating crystal breaking and uniform cooling operation.
Description
The technical field is as follows:
the invention relates to the technical field of vegetable oil processing, in particular to a coconut oil catalytic crystal growing and fractionation method.
Background art:
coconut oil is one of four edible woody oils in the world and is a main woody oil crop and food energy source in tropical regions. Coconut trees grow on islands in tropical regions or along continents, mainly concentrated in the southeast asia. Coconut has more than 2000 years of cultivation history in China, is mainly produced in Hainan island, and is partially planted in Leizhou peninsula, Yunnan province and Taiwan province.
Coconut oil is the major coconut-processed product worldwide. Coconut oil is also called coconut oil, and is obtained from coconut meat or dried coconut, and is white or light yellow fat. The coconut meat or the dried coconut contains 65 to 74 percent of oil and 4 to 7 percent of water. Coconut oil is a good health food material because of its special fatty acid composition and active substances with various physiological functions, and the coconut oil contains about 50% of lauric acid (C12) and about 15% of other medium-short carbon-chain fatty acids (caprylic acid C8 and capric acid C10), and is the most main source of lauric acid and medium-short chain fatty acids in the plant world.
Coconut oil is a tropical oil, has a high melting point, is semisolid at normal temperature, and is generally processed into products with different melting points by a fractionation method so as to meet the use requirements of different consumers. The coconut oil can be fractionated to obtain coconut liquid oil, coconut stearin, coconut special oil, etc.
The fractionation method of coconut oil generally comprises three methods, namely crystal growing fractionation, liquid-liquid extraction and distillation fractionation. The method is an economic and environment-friendly method, does not add any solvent, completely dissolves the coconut oil by heating, then carries out gradient cooling, and then carries out filtration separation on solid and liquid coconut oil. The crystal growing and fractionation can be divided into three steps: heating for breaking crystal, cooling to form crystal, and filtering for separation to obtain low-melting-point liquid phase (liquid coconut oil) and high-melting-point solid phase (solid coconut oil). The key process is that cooling promotes the stable growth of the crystal, if the crystallization process is smooth, the crystal is compact without excessive liquid wrapping, and the later separation is easy. The general crystal growing fractionation has difficulties or defects, namely, when coconut oil is cooled, because initially formed crystals are unstable, low-melting-point liquid oil in the growth process can be attached to high-melting-point solids, namely, the crystals contain a large amount of low-melting-point components, the quality and yield of final fractionation components are influenced, the sizes of crystal particles obtained by the initial crystal growing fractionation are irregular, the crystal particles are slow and uncontrolled, the separation of liquid fat and hard fat in the crystal growing fractionation is very difficult, the fractionation time is too long, and the problems of the separation in the initial stage and the later stage of the crystal growth cannot be fundamentally solved.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a coconut oil catalytic crystal growing and separating method, which not only can effectively control the cooling and crystallizing process of grease, but also can ensure that the crystal shape and size are uniform.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a coconut oil catalytic crystal growing and fractionation method comprises the following steps:
(1) heating and breaking crystal: heating the coconut oil under stirring to destroy the disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 20-25 ℃ at a cooling speed of 0.5-2.5 ℃/min and preserving heat for 0.5-2 h;
(3) first small-amplitude uniform temperature rise: adding seed crystals into the coconut oil cooled in the step (2), heating to 30-35 ℃ at a heating rate of 0.05-0.5 ℃/min, and keeping the temperature for 0.5-2 h;
(4) first small-amplitude uniform cooling: cooling the coconut oil heated in the step (3) to 10-15 ℃ at a cooling speed of 0.05-0.5 ℃/min and preserving heat for 0.5-2 h;
(5) and (3) small-amplitude uniform temperature rise for the second time: heating the coconut oil cooled in the step (4) to 20-25 ℃ at a heating rate of 0.05-0.5 ℃/min, and keeping the temperature for 0.5-2 h;
(6) and (3) small-amplitude uniform cooling for the second time: cooling the coconut oil heated in the step (5) to 10-15 ℃ at a cooling speed of 0.05-0.5 ℃/min and preserving heat for 0.5-2 h;
(7) sampling and detecting: during detection, the sample is filtered, when the iodine value of the filtrate of the sample meets the target requirement, the filter pressing is carried out by a diaphragm, the obtained filtrate is the liquid coconut oil, and the obtained filter residue is the solid coconut oil.
The iodine value of the coconut oil in the step (1) is 6.3-10.6g/100 g.
The heating temperature in the step (1) is 60-70 ℃.
The adding amount of the seed crystal in the step (3) accounts for 0.5-5% of the mass of the coconut oil serving as the raw material.
The seeds in step (3) were fluid and solid crystalline coconut oil was visible.
According to the technical scheme, the cooling time is shortened by adopting a large-amplitude uniform cooling mode before crystal nuclei are not formed, the formation of the crystal nuclei is stimulated by the first small-amplitude uniform cooling, the growth of the crystal nuclei is promoted by the first small-amplitude uniform cooling at the initial stage of the formation of the crystal nuclei, the shape and the size of the formed crystals tend to be uniform and the influence on subsequent filter pressing separation caused by the rapid aggregation of the crystals is avoided by the second small-amplitude uniform cooling after a large number of crystals appear, and finally the crystal form is completely changed from α type to β' type by the second small-amplitude uniform cooling.
Compared with the existing coconut oil fractionation method, the technical scheme can obviously shorten fractionation time and reduce fractionation cost, but the obtained technical effect is still not ideal, so in order to further optimize the technical effect, the technical problem to be solved by the invention can be realized by adopting the following technical scheme:
a coconut oil catalytic crystal growing and fractionation method comprises the following steps:
(1) heating and breaking crystal: heating the coconut oil under stirring to destroy the disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: adding a crystallization promoter into the coconut oil subjected to crystal breaking in the step (1), cooling to 20-25 ℃ at a cooling speed of 0.5-2.5 ℃/min, performing filter pressing to remove the crystallization promoter, and then preserving heat at 20-25 ℃ for 0.5-2 h;
(3) small uniform cooling: cooling the coconut oil cooled in the step (2) to 10-15 ℃ at a cooling speed of 0.05-0.5 ℃/min and preserving heat for 2-5 h;
(4) sampling and detecting: during detection, the sample is filtered, when the iodine value of the filtrate of the sample meets the target requirement, the filter pressing is carried out by a diaphragm, the obtained filtrate is the liquid coconut oil, and the obtained filter residue is the solid coconut oil.
The iodine value of the coconut oil in the step (1) is 6.3-10.6g/100 g.
The heating temperature in the step (1) is 60-70 ℃.
The addition amount of the crystallization accelerator in the step (2) accounts for 0.5-5% of the mass of the raw coconut oil.
And (3) the crystallization promoter in the step (2) is magnesium aluminum silicate.
The crystallization accelerant in the step (2) is zinc dimethacrylate.
The inventor unexpectedly finds that the forming time of crystal nucleus can be obviously shortened and the growth speed of the crystal nucleus can be accelerated when the magnesium aluminum silicate or the zinc dimethacrylate is used as the crystallization promoter in many years of research, and the formed crystal has uniform shape and size; the invention removes the crystallization promoter through pressure filtration operation before the crystals are formed in large quantity, so as to avoid the crystallization promoter from being wrapped in the crystals and difficult to separate from the crystals.
The invention has the beneficial effects that: the invention can effectively control the cooling and crystallizing process of the oil, can ensure that the crystal shape and the size are uniform, adopts a relatively quick cooling mode to shorten the crystallization and cooling time of the coconut oil, more fully separates the solid and the liquid after fractionation of the coconut oil, effectively controls the temperature return during fractionation, and improves the product quality of the coconut oil.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 25 ℃ at a cooling speed of 2 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(3) first small-amplitude uniform temperature rise: under the stirring speed of 20r/min, adding 2.5g of seed crystal into the coconut oil cooled in the step (2), wherein the seed crystal is fluid and can see solid crystallized coconut oil, and heating to 32 ℃ at the heating speed of 0.25 ℃/min and preserving heat for 0.5 h;
(4) first small-amplitude uniform cooling: cooling the coconut oil heated in the step (3) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(5) and (3) small-amplitude uniform temperature rise for the second time: heating the coconut oil cooled in the step (4) to 22 ℃ at a heating rate of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(6) and (3) small-amplitude uniform cooling for the second time: cooling the coconut oil heated in the step (5) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 1h under the stirring speed of 20 r/min;
(7) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 9.5g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Example 2
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.8g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 25 ℃ at a cooling speed of 2 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(3) first small-amplitude uniform temperature rise: under the stirring speed of 20r/min, adding 2.5g of seed crystal into the coconut oil cooled in the step (2), wherein the seed crystal is fluid and can see solid crystallized coconut oil, and heating to 32 ℃ at the heating speed of 0.25 ℃/min and preserving heat for 0.5 h;
(4) first small-amplitude uniform cooling: cooling the coconut oil heated in the step (3) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(5) and (3) small-amplitude uniform temperature rise for the second time: heating the coconut oil cooled in the step (4) to 22 ℃ at a heating rate of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(6) and (3) small-amplitude uniform cooling for the second time: cooling the coconut oil heated in the step (5) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 1h under the stirring speed of 20 r/min;
(7) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 9.8g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that the first small-amplitude uniform temperature rise and the second small-amplitude uniform temperature rise are eliminated, the first small-amplitude uniform temperature drop and the second small-amplitude uniform temperature drop are combined into a small-amplitude uniform temperature drop, and the heat preservation time of the first small-amplitude uniform temperature rise and the second small-amplitude uniform temperature rise is added to the small-amplitude uniform temperature drop.
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 25 ℃ at a cooling speed of 2 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(3) small uniform cooling: under the stirring speed of 20r/min, adding 2.5g of seed crystal into the coconut oil cooled in the step (2), wherein the seed crystal is fluid and can see solid crystallized coconut oil, cooling to 12 ℃ at the cooling speed of 0.5 ℃/min, and preserving heat for 2.5 h;
(4) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 8.3g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Comparative example 2
Comparative example 2 differs from example 1 in that no seed crystal was added.
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 25 ℃ at a cooling speed of 2 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(3) first small-amplitude uniform temperature rise: heating to 32 ℃ at a heating rate of 0.25 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(4) first small-amplitude uniform cooling: cooling the coconut oil heated in the step (3) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(5) and (3) small-amplitude uniform temperature rise for the second time: heating the coconut oil cooled in the step (4) to 22 ℃ at a heating rate of 0.5 ℃/min and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(6) and (3) small-amplitude uniform cooling for the second time: cooling the coconut oil heated in the step (5) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 1h under the stirring speed of 20 r/min;
(7) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 8.0g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Example 3
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: stirring at 20r/min, adding 2.5g of magnesium aluminum silicate into the coconut oil subjected to crystal breaking in the step (1), cooling to 25 ℃ at the cooling rate of 2 ℃/min, performing filter pressing to remove the magnesium aluminum silicate, and keeping the temperature at 25 ℃ for 0.5 h;
(3) small uniform cooling: cooling the coconut oil cooled in the step (2) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 2.5h under the stirring speed of 20 r/min;
(4) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 10.3g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Example 4
Example 4 differs from example 3 in that the crystallisation accelerator is replaced by an equal amount of zinc dimethacrylate instead of magnesium aluminium silicate.
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: stirring at 20r/min, adding 2.5g zinc dimethacrylate into the coconut oil after crystal breaking in the step (1), cooling to 25 ℃ at the cooling rate of 2 ℃/min, removing the zinc dimethacrylate through pressure filtration, and keeping the temperature at 25 ℃ for 0.5 h;
(3) small uniform cooling: cooling the coconut oil cooled in the step (2) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 2.5h under the stirring speed of 20 r/min;
(4) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 10.0g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
Comparative example 3
Comparative example 3 is different from example 3 in that no crystallization promoter was added.
(1) Heating and breaking crystal: heating 500g of coconut oil with iodine value of 6.3g/100g to 65 ℃ at a stirring speed of 60r/min, and preserving heat for 1h to destroy disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) at a cooling speed of 2 ℃/min to 25 ℃ and keeping the temperature for 0.5h under the stirring speed of 20 r/min;
(3) small uniform cooling: cooling the coconut oil cooled in the step (2) to 12 ℃ at a cooling speed of 0.5 ℃/min and keeping the temperature for 2.5h under the stirring speed of 20 r/min;
(4) sampling and detecting: during detection, a sample is filtered, the iodine value of a filtrate of the sample is 7.7g/100g, and the filtrate is subjected to filter pressing by a diaphragm, namely liquid coconut oil, and filter residue is solid coconut oil.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A coconut oil catalytic crystal growing and fractionation method is characterized by comprising the following steps:
(1) heating and breaking crystal: heating the coconut oil under stirring to destroy the disordered crystal structure;
(2) greatly reducing the temperature at a constant speed: cooling the coconut oil after the crystal breaking in the step (1) to 20-25 ℃ at a cooling speed of 0.5-2.5 ℃/min and preserving heat for 0.5-2 h;
(3) first small-amplitude uniform temperature rise: adding seed crystals into the coconut oil cooled in the step (2), heating to 30-35 ℃ at a heating rate of 0.05-0.5 ℃/min, and keeping the temperature for 0.5-2 h;
(4) first small-amplitude uniform cooling: cooling the coconut oil heated in the step (3) to 10-15 ℃ at a cooling speed of 0.05-0.5 ℃/min and preserving heat for 0.5-2 h;
(5) and (3) small-amplitude uniform temperature rise for the second time: heating the coconut oil cooled in the step (4) to 20-25 ℃ at a heating rate of 0.05-0.5 ℃/min, and keeping the temperature for 0.5-2 h;
(6) and (3) small-amplitude uniform cooling for the second time: cooling the coconut oil heated in the step (5) to 10-15 ℃ at a cooling speed of 0.05-0.5 ℃/min and preserving heat for 0.5-2 h;
(7) sampling and detecting: during detection, the sample is filtered, when the iodine value of the filtrate of the sample meets the target requirement, the filter pressing is carried out by a diaphragm, the obtained filtrate is the liquid coconut oil, and the obtained filter residue is the solid coconut oil.
2. The coconut oil catalytic crystal growing and fractionation method according to claim 1, characterized in that: the iodine value of the coconut oil in the step (1) is 6.3-10.6g/100 g.
3. The coconut oil catalytic crystal growing and fractionation method according to claim 1, characterized in that: the heating temperature in the step (1) is 60-70 ℃.
4. The coconut oil catalytic crystal growing and fractionation method according to claim 1, characterized in that: the adding amount of the seed crystal in the step (3) accounts for 0.5-5% of the mass of the coconut oil serving as the raw material.
5. The coconut oil catalytic crystal growing and fractionation method according to claim 1, characterized in that: the seeds in step (3) were fluid and solid crystalline coconut oil was visible.
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| CN112812886A (en) * | 2020-12-31 | 2021-05-18 | 海南大学 | Preparation method of low-melting-point coconut oil |
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| CN101697757A (en) * | 2009-10-23 | 2010-04-28 | 福建印福油脂工业有限公司 | Dry fractionation method for palm oil |
| CN102604739A (en) * | 2012-03-23 | 2012-07-25 | 天津龙威粮油工业有限公司 | Method for dry fractionation of palm oil |
| CN103614239A (en) * | 2013-12-05 | 2014-03-05 | 天津大学 | Method for preparing low-temperature-resistant palm oil with high iodine value |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697757A (en) * | 2009-10-23 | 2010-04-28 | 福建印福油脂工业有限公司 | Dry fractionation method for palm oil |
| CN102604739A (en) * | 2012-03-23 | 2012-07-25 | 天津龙威粮油工业有限公司 | Method for dry fractionation of palm oil |
| CN103614239A (en) * | 2013-12-05 | 2014-03-05 | 天津大学 | Method for preparing low-temperature-resistant palm oil with high iodine value |
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