CN111548855A - Five-threshing process of linseed crude oil - Google Patents
Five-threshing process of linseed crude oil Download PDFInfo
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- CN111548855A CN111548855A CN202010380400.5A CN202010380400A CN111548855A CN 111548855 A CN111548855 A CN 111548855A CN 202010380400 A CN202010380400 A CN 202010380400A CN 111548855 A CN111548855 A CN 111548855A
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- crude oil
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- linseed
- crude
- deacidified
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- 239000010779 crude oil Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 53
- 235000004426 flaxseed Nutrition 0.000 title claims abstract description 18
- 235000004431 Linum usitatissimum Nutrition 0.000 title abstract description 15
- 240000006240 Linum usitatissimum Species 0.000 title abstract description 15
- 235000021388 linseed oil Nutrition 0.000 claims abstract description 37
- 239000000944 linseed oil Substances 0.000 claims abstract description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 230000001939 inductive effect Effects 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 230000001877 deodorizing effect Effects 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- MJYQFWSXKFLTAY-OVEQLNGDSA-N (2r,3r)-2,3-bis[(4-hydroxy-3-methoxyphenyl)methyl]butane-1,4-diol;(2r,3r,4s,5s,6r)-6-(hydroxymethyl)oxane-2,3,4,5-tetrol Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O.C1=C(O)C(OC)=CC(C[C@@H](CO)[C@H](CO)CC=2C=C(OC)C(O)=CC=2)=C1 MJYQFWSXKFLTAY-OVEQLNGDSA-N 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims 2
- 230000008025 crystallization Effects 0.000 claims 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 238000007670 refining Methods 0.000 abstract description 10
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 abstract description 7
- 235000020661 alpha-linolenic acid Nutrition 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 7
- 229960004488 linolenic acid Drugs 0.000 abstract description 7
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 6
- 150000002978 peroxides Chemical class 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000003921 oil Substances 0.000 abstract description 4
- 235000019198 oils Nutrition 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004332 deodorization Methods 0.000 description 3
- 239000003957 anion exchange resin Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a five-step process for linseed crude oil. Compared with the prior art, the invention has the following beneficial effects: (1) the five-threshing process of the linseed crude oil is simple in process, convenient to operate, low in process cost, high in refining yield, good in product quality and suitable for industrial production; (2) the refined yield of the finished product oil of the linseed oil obtained by refining by utilizing the five-threshing process of the crude linseed oil is higher than 98.97%, the loss rate of linolenic acid is lower than 0.55%, the acid value is lower than 0.11KOHmg/g, the peroxide value is lower than 0.45mmlo/kg, the moisture content is 0.02% and the impurity content is 0.03%.
Description
Technical Field
The invention belongs to the technical field of vegetable oil refining, relates to a refining treatment process of linseed oil, and particularly relates to a five-threshing process of crude linseed oil.
Background
The linseed oil is prepared from linseed, wherein the oil content of the linseed is up to 30-35%, the linolenic acid accounts for 45-60% of the oil content, and the linoleic acid is a functional active substance and has high utilization value in various health-care foods.
Most of linseed oil is physically squeezed or chemically extracted, but the extracted crude oil contains a large amount of impurities, the flavor and the character of the linseed oil are influenced, the product quality is greatly influenced, and further the product sale is influenced.
In order to better improve the product quality, most of the existing refining methods of crude linseed oil only adopt deacidification and decolorization or only adopt deacidification and deodorization, so that the production cost is low, but the finished product is not refined enough and has poor quality, and meanwhile, after the refining, the moisture content and impurity content are high, the loss rate of linolenic acid is also high, so that the refining methods are very unfavorable for industrial production.
In view of this, this patent is filed.
Disclosure of Invention
In order to overcome the defects of the prior art, simplify the process method, reduce the production cost and improve the product quality, the invention provides a five-threshing process of crude linseed oil by taking the crude linseed oil as a raw material. The five-removal process comprises five steps of deacidification, degumming, decoloration, deodorization and dewaxing, and the refined yield of the finished oil prepared by the process method is higher than 98.97%, the loss rate of linolenic acid is lower than 0.55%, the acid value is lower than 0.11KOHmg/g, the peroxide value is lower than 0.45mmlo/kg, the moisture content is 0.02% and the impurity content is 0.03%.
The invention aims to provide a five-threshing process of linseed crude oil.
According to the present invention, the method for five-step removing of crude linseed oil comprises:
(1) deacidifying: mixing raw linseed oil crude oil with a sodium hydroxide aqueous solution at 80 ℃, centrifuging, and taking an upper layer liquid to obtain deacidified crude oil;
(2) degumming: washing the deacidified crude oil obtained in the step (1) with water at 80 ℃, centrifuging, and taking the upper-layer liquid to obtain degummed crude oil;
(3) and (3) decoloring: adding activated carbon into the degummed crude oil obtained in the step (2) at the temperature of 100-120 ℃, filtering and taking filtrate to obtain decolorized crude oil;
(4) deodorizing: performing vacuum steam treatment at 230 ℃ to obtain deodorized crude oil;
(5) dewaxing: and (3) adding a crystal inducing agent into the deodorized crude oil obtained in the step (4) at 0 ℃, fully stirring, filtering solids, and taking liquid to obtain refined linseed oil.
According to the five-removal process of the linseed crude oil, the adding amount of the sodium hydroxide aqueous solution in the step (1) is 0.5-2% by mass percent.
According to the five-removal process of the linseed crude oil, the mass concentration of the sodium hydroxide aqueous solution in the step (1) is 2% -5%.
According to the five-step process for crude linseed oil according to the specific embodiment of the invention, in the step (2), deacidified crude oil is washed with water and then centrifuged, and the obtained upper-layer liquid is washed with water again and then centrifuged to obtain degummed crude oil.
According to the five-step process of the crude linseed oil according to the embodiment of the invention, in the step (2), the water consumption of the water washing is more than 5 times of the volume of the deacidified crude oil.
According to the five-threshing process of the linseed crude oil provided by the embodiment of the invention, in the step (3), the using amount of the activated carbon is 12% -15%.
According to the five-threshing process of the crude linseed oil, in the step (3), the degummed crude linseed oil and the activated carbon are mixed and stirred for 0.5-1 hour.
According to the five-step process of flaxseed crude oil, in the step (4), steam is introduced from the bottom of the decolorized crude oil obtained in the step (3) for 1-3 hours.
According to the five-threshing process of crude linseed oil according to the specific embodiment of the invention, in the step (5), the crystal inducing agent is diatomite.
According to the five-threshing process of the linseed crude oil provided by the embodiment of the invention, in the step (5), the addition amount of the crystal inducing agent is 0.5-2% by mass.
Compared with the prior art, the invention has the following beneficial effects:
(1) the five-threshing process of the linseed crude oil is simple in process, convenient to operate, low in process cost, high in refining yield, good in product quality and suitable for industrial production;
(2) the five-removal process of the crude linseed oil comprises five steps of deacidification, degumming, decoloration, deodorization and dewaxing, the refined linseed oil has finished products meeting the regulations of GB/T8235-2008 linseed oil, good quality, better color and acid value than common edible oil, difficult oxidation, easier storage, fragrant smell and no scorched bitter taste, and the refined yield of the finished linseed oil is higher than 98.97%, the loss rate of linolenic acid is lower than 0.55%, the acid value is lower than 0.11KOHmg/g, the peroxide value is lower than 0.45mmlo/kg, the moisture content is 0.02% and the impurity content is 0.03%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The raw materials adopted in the invention are pretreatment products of an upstream process, and the treatment method is the prior art and is not described herein again; sodium hydroxide, active carbon and diatomite are all commercially available products in the process.
Example 1
The embodiment provides a five-threshing process of linseed crude oil, which comprises the following steps:
(1) deacidifying: mixing raw linseed oil crude oil with a sodium hydroxide aqueous solution at 80 ℃, centrifuging, and taking an upper layer liquid to obtain deacidified crude oil; wherein the addition amount of the sodium hydroxide aqueous solution is 0.5 percent by mass, and the mass concentration of the sodium hydroxide aqueous solution is 2 percent;
(2) degumming: washing the deacidified crude oil obtained in the step (1) with water at 80 ℃, centrifuging, washing the obtained upper layer liquid again, and centrifuging to obtain degummed crude oil; wherein, the water consumption of each time of water washing is more than 6 times of the volume of the deacidified crude oil;
(3) and (3) decoloring: adding activated carbon into the degummed crude oil obtained in the step (2) at 100 ℃, stirring for 0.h, filtering, and taking filtrate to obtain decolorized crude oil; the using amount of the active carbon is 12 percent by mass;
(4) deodorizing: introducing steam from the bottom of the decolored crude oil obtained in the step (3) at 230 ℃ in a vacuum environment for 1 hour to obtain deodorized crude oil;
(5) dewaxing: and (3) adding diatomite into the deodorized crude oil obtained in the step (4) at 0 ℃, wherein the adding amount of the diatomite is 0.5 percent by mass, fully stirring, filtering solids, and taking liquid to obtain refined linseed oil.
Example 2
The embodiment provides a five-threshing process of linseed crude oil, which comprises the following steps:
(1) deacidifying: mixing raw linseed oil crude oil with a sodium hydroxide aqueous solution at 80 ℃, centrifuging, and taking an upper layer liquid to obtain deacidified crude oil; wherein the addition amount of the sodium hydroxide aqueous solution is 2 percent by mass, and the mass concentration of the sodium hydroxide aqueous solution is 5 percent;
(2) degumming: washing the deacidified crude oil obtained in the step (1) with water at 80 ℃, centrifuging, washing the obtained upper layer liquid again, and centrifuging to obtain degummed crude oil; wherein, the water consumption of each time of water washing is more than 7 times of the volume of the deacidified crude oil;
(3) and (3) decoloring: adding activated carbon into the degummed crude oil obtained in the step (2) at 120 ℃, stirring for 1 hour, and filtering to obtain filtrate to obtain decolorized crude oil; the using amount of the active carbon is 15 percent by mass;
(4) deodorizing: introducing steam from the bottom of the decolored crude oil obtained in the step (3) at 230 ℃ in a vacuum environment for 3 hours to obtain deodorized crude oil;
(5) dewaxing: and (3) adding diatomite into the deodorized crude oil obtained in the step (4) at 0 ℃, wherein the adding amount of the diatomite is 2 percent by mass, fully stirring, filtering solids, and taking liquid to obtain refined linseed oil.
Example 3
The embodiment provides a five-threshing process of linseed crude oil, which comprises the following steps:
(1) deacidifying: mixing raw linseed oil crude oil with a sodium hydroxide aqueous solution at 80 ℃, centrifuging, and taking an upper layer liquid to obtain deacidified crude oil; wherein the addition amount of the sodium hydroxide aqueous solution is 1 percent by mass, and the mass concentration of the sodium hydroxide aqueous solution is 3 percent;
(2) degumming: washing the deacidified crude oil obtained in the step (1) with water at 80 ℃, centrifuging, washing the obtained upper layer liquid again, and centrifuging to obtain degummed crude oil; wherein, the water consumption of each time of water washing is more than 8 times of the volume of the deacidified crude oil;
(3) and (3) decoloring: adding activated carbon into the degummed crude oil obtained in the step (2) at 110 ℃, stirring for 0.8 hour, filtering, and taking filtrate to obtain decolorized crude oil; the using amount of the active carbon is 13 mass percent;
(4) deodorizing: introducing steam from the bottom of the decolored crude oil obtained in the step (3) at 230 ℃ in a vacuum environment for 2 hours to obtain deodorized crude oil;
(5) dewaxing: and (3) adding diatomite into the deodorized crude oil obtained in the step (4) at 0 ℃, wherein the adding amount of the diatomite is 1 percent by mass, fully stirring, filtering solids, and taking liquid to obtain refined linseed oil.
Comparative example 1
The only difference between this comparative example and example 3 is that: and (3) decoloring by adopting macroporous anion exchange resin.
Comparative example 2
The only difference between this comparative example and example 3 is that: and (5) the crystal inducing agent adopted in the dewaxing in the step (5) is bentonite.
Performance test
The test method comprises the following steps: the performance of the refined linseed oil obtained in examples 1 to 4, comparative example 1 and comparative example 2 was tested, and the indexes of the finished linseed oil were determined according to the method specified in the standard GB/T8235-2008 "linseed oil", and the results are shown in table 1:
TABLE 1 linseed oil performance results
| Performance of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Refining yield (%) | 98.97 | 99.11 | 99.25 | 99.18 | 98.03 |
| Linolenic acid loss Rate (%) | 0.55 | 0.44 | 0.45 | 0.48 | 0.68 |
| Acid value (KOHmg/g) | 0.11 | 0.09 | 0.10 | 0.12 | 0.10 |
| Peroxide number (mmlo/kg) | 0.45 | 0.43 | 0.40 | 0.41 | 0.50 |
| Moisture content (%) | 0.02 | 0.02 | 0.02 | 0.03 | 0.05 |
| Content of impurities (%) | 0.03 | 0.03 | 0.03 | 0.03 | 0.05 |
As can be seen from the above table, the indexes of the refining yield, the linolenic acid loss rate, the acid value, the peroxide value, the moisture content and the impurity content of the examples 1 to 3 and the comparative example 1 are all good, but the cost of the macroporous anion exchange resin is high, the resin treatment process is complicated, and the time cost and the treatment cost are both high, so that under the same effect, the process cost of the invention is lower, and the method is more suitable for industrial production; the indexes of the comparative example 2 are all worse, so the process method of the invention is more beneficial to be selected.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A five-threshing process of crude linseed oil is characterized by comprising the following steps:
(1) deacidifying: mixing raw linseed oil crude oil with a sodium hydroxide aqueous solution at 80 ℃, centrifuging, and taking an upper layer liquid to obtain deacidified crude oil;
(2) degumming: washing the deacidified crude oil obtained in the step (1) with water at 80 ℃, centrifuging, and taking the upper-layer liquid to obtain degummed crude oil;
(3) and (3) decoloring: adding activated carbon into the degummed crude oil obtained in the step (2) at the temperature of 100-120 ℃, filtering and taking filtrate to obtain decolorized crude oil;
(4) deodorizing: performing vacuum steam treatment at 230 ℃ to obtain deodorized crude oil;
(5) dewaxing: and (3) adding a crystal inducing agent into the deodorized crude oil obtained in the step (4) at 0 ℃, fully stirring, filtering solids, and taking liquid to obtain refined linseed oil.
2. The process of claim 1, wherein in step (1), the amount of the aqueous solution of sodium hydroxide is 0.5-2% by mass.
3. The process of claim 1, wherein in the step (1), the concentration of the aqueous solution of sodium hydroxide is 2-5% by mass.
4. The five-delipidation process of crude linseed oil according to claim 1, wherein in the step (2), the deacidified crude oil is washed with water and then centrifuged, and the obtained upper liquid is washed with water again and then centrifuged to obtain the degummed crude oil.
5. The process of claim 1, wherein the water used in the step (2) is more than 5 times the volume of the deacidified crude oil.
6. The five-threshing process of flaxseed crude oil according to claim 1, wherein in step (3), the amount of activated carbon is 12-15%.
7. The five-threshing process of crude linseed oil according to claim 1, characterized in that in the step (3), the degummed crude oil is mixed with activated carbon and stirred for 0.5-1 hour.
8. The process of claim 1, wherein in step (4), steam is introduced from the bottom of the decolorized crude oil obtained in step (3) for 1-3 hours.
9. The process of claim 1, wherein in step (5), the crystallization inducing agent is diatomaceous earth.
10. The five-threshing process of flaxseed crude oil according to claim 1, wherein in step (5), the addition amount of the crystallization inducing agent is 0.5-2% by mass.
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| CN202010380400.5A CN111548855A (en) | 2020-05-08 | 2020-05-08 | Five-threshing process of linseed crude oil |
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| CN202010380400.5A CN111548855A (en) | 2020-05-08 | 2020-05-08 | Five-threshing process of linseed crude oil |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045356A (en) * | 2012-12-28 | 2013-04-17 | 邯郸晨光珍品油脂有限公司 | Production method for linseed oil |
| CN107090351A (en) * | 2017-04-13 | 2017-08-25 | 荣海生物科技有限公司 | A kind of linseed oil method of refining |
| CN107523415A (en) * | 2017-10-20 | 2017-12-29 | 烟台新时代健康产业有限公司 | A kind of preparation method of high-quality linseed oil |
| CN107557149A (en) * | 2016-06-30 | 2018-01-09 | 吴忠市兴达粮油有限公司 | A kind of siritch raw oil refining technique |
| CN108659954A (en) * | 2018-04-09 | 2018-10-16 | 浙江省农业科学院 | A kind of production method of tea seeds refined oil |
-
2020
- 2020-05-08 CN CN202010380400.5A patent/CN111548855A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045356A (en) * | 2012-12-28 | 2013-04-17 | 邯郸晨光珍品油脂有限公司 | Production method for linseed oil |
| CN107557149A (en) * | 2016-06-30 | 2018-01-09 | 吴忠市兴达粮油有限公司 | A kind of siritch raw oil refining technique |
| CN107090351A (en) * | 2017-04-13 | 2017-08-25 | 荣海生物科技有限公司 | A kind of linseed oil method of refining |
| CN107523415A (en) * | 2017-10-20 | 2017-12-29 | 烟台新时代健康产业有限公司 | A kind of preparation method of high-quality linseed oil |
| CN108659954A (en) * | 2018-04-09 | 2018-10-16 | 浙江省农业科学院 | A kind of production method of tea seeds refined oil |
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