CN104250582A - Method for extracting odorless white silkworm chrysalis oil from silkworm chrysalis leftover - Google Patents
Method for extracting odorless white silkworm chrysalis oil from silkworm chrysalis leftover Download PDFInfo
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- CN104250582A CN104250582A CN201410447485.9A CN201410447485A CN104250582A CN 104250582 A CN104250582 A CN 104250582A CN 201410447485 A CN201410447485 A CN 201410447485A CN 104250582 A CN104250582 A CN 104250582A
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Abstract
The invention discloses a method for extracting odorless white silkworm chrysalis oil from silkworm chrysalis leftover. The method comprises: drying and crushing silkworm chrysalis leftover, performing ultrasonic-assisted extraction of crude silkworm chrysalis oil by employing an organic solvent, adding modified graphene oxide into the obtained crude silkworm chrysalis oil, and performing adsorption processing and filtering, so as to obtain the odorless white refined silkworm chrysalis oil. The method is simple and rapid in operation, satisfies industrialized production. The prepared refined silkworm chrysalis oil is odorless and good in decoloring effect, and free of damage to effective compositions, and has important application value.
Description
Technical field
The present invention relates to a kind of method extracting odorless white silkworm chrysalis oil from silkworm chrysalis tankage, belong to bio oil manufacture field.
Background technology
Silkworm chrysalis is the principal by product of silk reeling industry, and producing one ton of raw silk can by-product one ton of dry pupa, its fat content about 30%.Silkworm chrysalis oil is rich in the unsaturated fatty acids of the lipid acid particularly multiple needed by human such as oleic acid, linoleic acid plus linolenic acid, there is high nutritive value, oleic acid wherein can reduce the LDL (low density cholesterol) in body effectively, has the effect of prevention of arterial sclerosis; Linolic acid is also the important substance sustained life, gamma-linolenic acid, DH-gamma linolenic acid and arachidonic acid can be changed in vivo, then synthesis of prostaglandins, can effectively Cardiovarscular, prevention myocardial infarction, linolic acid simultaneously can also with cholesterol esterification, reduce serum, liver and blood cholesterol levels in body, the formation of atherosclerosis and arterial thrombus; Alpha-linolenic acid can extend the meta-bolitess such as synthesis eicosa-pentaenoic (EPA), 22 carbon six (DHA) through dehydrogenation and carbochain in vivo; it is the life core substance maintaining the evolution of mankind's brain; there is several functions such as increasing intelligence, vision protection, delay senility; effectively can suppress thrombotic diseases; prevention myocardial infarction, cerebral infarction; reducing blood-fat, hypotensive, suppress hemorrhagic cerebral apoplexy, the generation suppressing cancer and transfer, prevention and prohibition senile dementia etc.
But the silkworm chrysalis oil extracted from silkworm chrysalis is dun and has strong peculiar smell, if do not removed, directly as food be difficult to accept, even if as animal-feed, also can remain in animal meat, birds, beasts and eggs, limit its development and utilization.There is no the problem that good method removes silkworm chrysalis oil bad smell at present, this hampers the application of silkworm chrysalis oil in field of health care products greatly.
At present, the method for silkworm chrysalis oil deodorization decoloring mainly contains following three kinds: H
2o
2oxidation style, organic solvent pickling process and active carbon adsorption.H
2o
2oxidation style decolorizing effect is better, and H
2o
2have the advantage of thermal degradation Cheng Shui, but its amino acid is subject to havoc, the security of applying its product in food is queried; Organic solvent pickling process can only remove oleophylic, lower boiling malodoring substance, and deodorization decoloring effect is undesirable.Gac is better to other method in silkworm chrysalis oil deodorization decoloring effect hinge structure, but gac is separated very difficult from silkworm chrysalis oil, cause the subsequent disposal of decolouring and deodorizing very difficult, and adsorption losses rate is larger.
Summary of the invention
De-oiling decoloration process for silkworm chrysalis oil of the prior art exists can not the defects such as simultaneously de-oiling and decolouring, destruction oil, aftertreatment be difficult, the object of the invention is to be that provide a kind of extracts thick silkworm chrysalis oil from silkworm chrysalis tankage, and utilize modified graphite oxide to carry out efficient decolouring and deodorization simultaneously to thick silkworm chrysalis oil, and do not affect oil, extract the method for high-quality odorless white silkworm chrysalis oil, the method flow process is short, simple to operate, cost is low, meets suitability for industrialized production.
The invention provides a kind of method extracting odorless white silkworm chrysalis oil from silkworm chrysalis tankage, the method is by after the oven dry of silkworm chrysalis tankage, pulverizing, adopt the thick silkworm chrysalis oil of ultrasonic wave added organic solvent extraction, modified graphene oxide is added by solid-to-liquid ratio 0.1 ~ 0.6g:10mL in the thick silkworm chrysalis oil of gained, adsorption treatment 0.25 ~ 5h is carried out under the temperature condition of 10 ~ 60 DEG C, filter, obtain the refining silkworm chrysalis oil of odorless white; Described modified graphene oxide by after 880 ~ 920 DEG C of pyroprocessing, adopts Hummers method to prepare by Graphite Powder 99.
The method extracting odorless white silkworm chrysalis oil from silkworm chrysalis tankage of the present invention also comprises following preferred version:
In preferred scheme, the solid-liquid mass volume ratio of modified graphene oxide and thick silkworm chrysalis oil is 0.2 ~ 0.5g:10mL.
In preferred scheme, the temperature of adsorption treatment is 15 ~ 40 DEG C.
In preferred scheme, the time of adsorption treatment is 1.8 ~ 2.5h.
In preferred scheme, modified graphite oxide joins in thick silkworm chrysalis oil and carries out batch type, makes decoloration and deodorization more complete.
In preferred scheme, Graphite Powder 99 is 10 ~ 20s in the time of 880 ~ 920 DEG C of pyroprocessing.
Drying in preferred scheme is silkworm chrysalis is dried biodiversity content under 55 ~ 65 DEG C of conditions to be not more than 5%.
In preferred scheme, silkworm chrysalis is crushed to granularity within the scope of-40 order ~+60 objects after drying.
In preferred scheme, organic solvent is the mixed solvent of sherwood oil and hexanaphthene.Described sherwood oil and hexamethylene ring are preferably 0.5 ~ 1.5:1 mixing by volume.
Further preferred scheme: silkworm chrysalis is dried under 55 ~ 65 DEG C of conditions after biodiversity content is not more than 5%, be crushed to granularity within the scope of-40 order ~+60 objects; Pulverizing the silkworm chrysalis powder obtained adopts the mixed solvent of sherwood oil and hexanaphthene to carry out refluxing extraction under the condition of ultrasonic wave added, obtain thick silkworm chrysalis oil, modified graphene oxide is added by solid-to-liquid ratio 0.2 ~ 0.5g:10mL in the thick silkworm chrysalis oil of gained, carry out adsorption treatment 1.8 ~ 2.5h at 15 ~ 40 DEG C of temperature after, filter, obtain the refining silkworm chrysalis oil of odorless white.
Best adsorption treatment scheme is adsorption temp is 30 DEG C, and the time is 2h, and the mass volume ratio of modified graphene oxide and silkworm chrysalis oil silkworm chrysalis oil is roughly 0.2g:10mL.
Compared with prior art, the present invention has following beneficial effect:
1, the deodorization decoloring while that the present invention adopting modified graphene oxide to carry out thick silkworm chrysalis oil first, its percent of decolourization reaches 72.45%, and simultaneously good deodorization effect, the refining silkworm chrysalis oil free from extraneous odour obtained, and after thick silkworm chrysalis oil deodorization decoloring, modified graphene oxide without impact, obtains high-quality silkworm chrysalis oil on the oil of silkworm chrysalis oil.
2, the while that modified graphene oxide of the present invention carrying out thick silkworm chrysalis oil, the technique of deodorization decoloring is simple especially, do not need special equipment and reagent, only modified graphene oxide need be added in thick silkworm chrysalis oil, place for some time (intermittent stirring several times).
3, the present invention adopt modified graphene oxide to make sorbent material not only decoloration and deodorization is effective, and be easy to be separated with silkworm chrysalis oil, aftertreatment is simple.
4, reaction conditions when the present invention adopts modified graphene oxide to carry out deodorization decoloring is gentle, and treatment temp is low, and the time is short, and other composition in oil can not be destroyed by high temperature oxidation.
Embodiment
Following examples are intended to further illustrate content of the present invention, and protection scope of the present invention does not limit by embodiment.
The preparation of the modified graphene oxide adopted in the embodiment of the present invention:
First take 2.0g Graphite Powder 99 in large porcelain boat, after the high temperature Muffle furnace subsequently porcelain boat being placed in 900 DEG C leaves standstill the time of 15s, take out that to be cooled to room temperature for subsequent use, next takes 1.0g SODIUMNITRATE in 500mL round-bottomed flask, and adds 46mL 98% vitriol oil wherein, makes the temperature of its reaction system maintain 0 DEG C, and stirs until SODIUMNITRATE is dissolved in sulphuric acid soln completely, after will Graphite Powder 99 stir under join in reaction solution, add rear continuations stirring 30min, next 6g potassium permanganate is taken, slowly join in round-bottomed flask, and stir, after potassium permanganate all adds, continue to be stirred to reaction soln become blackish green till, now round-bottomed flask being proceeded to prior design temperature is react 4h under magnetic agitation in the oil bath pan of 35 DEG C, then in flask, slowly deionized water 92mL is dripped, be heated to 90 DEG C simultaneously, after deionization drips, after continuing to stir 30min, product is poured in 100mL beaker, and dilute with 124mL hot deionized water, finally use the process of 60mL 3% hydrogen peroxide, again by solution centrifugation while hot, with deionized water repetitive scrubbing product to neutral (pH=6.5-7).Finally modified graphene oxide (GO) is put into 60 DEG C of Constant Temp. Ovens, drying for standby.
Embodiment 1
1, extraction obtains thick silkworm chrysalis oil
First tankage silkworm chrysalis is dried at about 60 DEG C and pulverized, obtain water content and be less than 5%, granularity is-40 order ~+60 object dried silkworm chrysalis meals, and organic solvent is the mixing solutions of sherwood oil and hexanaphthene (1:1), then adopts ultrasonic-reflow method to extract and obtains thick silkworm chrysalis oil.
2, modified graphene oxide absorption
Get the thick silkworm chrysalis oil of 10mL, add 0.2g modified graphene oxide, then under 30 DEG C of conditions, process 2h, stir once therebetween every 20min, reaction terminates rear taking-up, filters, obtains the refining silkworm chrysalis oil of deodorization decoloring.Measure color, the smell of the rear silkworm chrysalis oil of process.Percent of decolourization is 71.83%, silkworm chrysalis oil odorless.
Embodiment 2
1, the method obtaining thick silkworm chrysalis oil is extracted identical with embodiment 1.
2, in the thick silkworm chrysalis oil of 10mL, 0.2g Powdered Activated Carbon and 0.2g modified graphene oxide is added respectively, 2h is processed under temperature 30 DEG C of conditions, stir once every 20min therebetween, reaction terminates rear taking-up, and measuring its percent of decolourization, the percent of decolourization of result gac is 52.74%, has residual odors, the percent of decolourization of modified graphene oxide is 71.83%, and odorless is remaining.
Embodiment 3
1, the method obtaining thick silkworm chrysalis oil is extracted identical with embodiment 1.
2, get the thick silkworm chrysalis oil of 10mL, add 0.2g modified graphene oxide, then under 30 DEG C of conditions, process 2h, stir once therebetween every 20min, reaction terminates rear taking-up, filters, obtains the refining silkworm chrysalis oil of deodorization decoloring.Measure silkworm chrysalis main body of oil before and after process with GC, result is as shown in table 1, as can be seen from the table, uses modified graphene oxide (GO) substantially not affect silkworm chrysalis oil quality as sorbent material.
Silkworm chrysalis main body of oil before and after table 1 processes
| Title | Palmiticacid | Stearic acid | Oleic acid | Linolic acid | Alpha-linolenic acid |
| Before process/% | 18.4256 | 7.7675 | 36.5279 | 4.8457 | 28.5623 |
| After decolouring/% | 18.1247 | 7.8542 | 36.6250 | 4.7526 | 28.4533 |
Embodiment 4
1, the method obtaining thick silkworm chrysalis oil is extracted identical with embodiment 1.
2, change temperature condition in adsorption process, other condition is identical with embodiment 1, and in 15 ~ 40 DEG C of temperature ranges, test result is as shown in table 2.
Table 2 temperature of reaction is on the impact of deodorization decoloring effect
Embodiment 5
1, the method obtaining thick silkworm chrysalis oil is extracted identical with embodiment 1.
2, change time conditions in adsorption process, other condition is identical with embodiment 1.In 0.25 ~ 5h time range, test result is as shown in table 3.
Table 3 treatment time is on the impact of decoloration and deodorization effect
Embodiment 6
1, the method obtaining thick silkworm chrysalis oil is extracted identical with embodiment 1.
2, change modified graphene oxide consumption condition in adsorption process, other condition is identical with embodiment 1.In the scope of the thick silkworm chrysalis oil of 0.1 ~ 0.6g modified graphene oxide/10mL, test result is as shown in table 4.
Table 4 modified graphene oxide (GO) consumption is on the impact of deodorization decoloring effect
The to sum up experimental data of embodiment 4 ~ 6, optimum experimental condition of the present invention is adsorption temp is 30 DEG C, and the time is 2h, and the mass volume ratio of modified graphene oxide and silkworm chrysalis oil silkworm chrysalis oil is roughly 0.2g:10mL.
Claims (8)
1. one kind is extracted the method for odorless white silkworm chrysalis oil from silkworm chrysalis tankage, it is characterized in that, after the oven dry of silkworm chrysalis tankage, pulverizing, adopt the thick silkworm chrysalis oil of ultrasonic wave added organic solvent extraction, modified graphene oxide is added by solid-to-liquid ratio 0.1 ~ 0.6g:10mL in the thick silkworm chrysalis oil of gained, under the temperature condition of 10 ~ 60 DEG C, carry out adsorption treatment 0.25 ~ 5h, filter, obtain the refining silkworm chrysalis oil of odorless white; Described modified graphene oxide by after 880 ~ 920 DEG C of pyroprocessing, adopts Hummers method to prepare by Graphite Powder 99.
2. the method for claim 1, is characterized in that, the solid-to-liquid ratio of graphene oxide and thick silkworm chrysalis oil is 0.2 ~ 0.5g:10mL.
3. the method for claim 1, is characterized in that, described adsorption treatment temperature is 15 ~ 40 DEG C.
4. the method for claim 1, is characterized in that, the described adsorption treatment time is 1.8 ~ 2.5h.
5. the method for claim 1, is characterized in that, described oven dry silkworm chrysalis is dried biodiversity content under 55 ~ 65 DEG C of conditions to be not more than 5%.
6. the method for claim 1, is characterized in that, silkworm chrysalis is crushed to granularity within the scope of-40 order ~+60 objects after drying.
7. the method for claim 1, is characterized in that, described organic solvent is the mixed solvent of sherwood oil and hexanaphthene.
8. the method as described in any one of claim 1 ~ 7, is characterized in that, is dried to by silkworm chrysalis after biodiversity content is not more than 5%, be crushed to granularity within the scope of-40 order ~+60 objects under 55 ~ 65 DEG C of conditions; Pulverizing the silkworm chrysalis powder obtained adopts the mixed solvent of sherwood oil and hexanaphthene to carry out refluxing extraction under the condition of ultrasonic wave added, obtain thick silkworm chrysalis oil, modified graphene oxide is added by solid-to-liquid ratio 0.2 ~ 0.5g:10mL in the thick silkworm chrysalis oil of gained, carry out adsorption treatment 1.8 ~ 2.5h at 15 ~ 40 DEG C of temperature after, filter, obtain the refining silkworm chrysalis oil of odorless white.
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| CN201410447485.9A CN104250582B (en) | 2014-09-04 | 2014-09-04 | A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis |
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| CN201410447485.9A CN104250582B (en) | 2014-09-04 | 2014-09-04 | A kind of method that odorless white silkworm chrysalis oil is extracted in the leftover bits and pieces from silkworm chrysalis |
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Citations (7)
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| CN101781601A (en) * | 2010-02-24 | 2010-07-21 | 陕西师范大学 | Method for extracting pupa oil from silkworm pupa by using ultrasonic wave |
| CN102965189A (en) * | 2012-11-09 | 2013-03-13 | 天津耀宇生物技术有限公司 | Method for extracting chrysalis oil |
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| CN102992305A (en) * | 2012-10-25 | 2013-03-27 | 中南大学 | Graphene material and preparation method of solid graphene |
| CN102504958B (en) * | 2011-11-03 | 2013-10-30 | 江苏科技大学 | Method for separating unsaturated fatty acids from silkworm chrysalis oil based on composition complexation of reversible reaction |
| CN103540394A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for extracting silkworm pupa oil by utilizing ultrasonic assisted aqueous enzymatic method |
| CN103540402A (en) * | 2013-10-31 | 2014-01-29 | 西南大学 | Method for reducing content of cholesterol in chrysalis oil |
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2014
- 2014-09-04 CN CN201410447485.9A patent/CN104250582B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781601A (en) * | 2010-02-24 | 2010-07-21 | 陕西师范大学 | Method for extracting pupa oil from silkworm pupa by using ultrasonic wave |
| CN102504958B (en) * | 2011-11-03 | 2013-10-30 | 江苏科技大学 | Method for separating unsaturated fatty acids from silkworm chrysalis oil based on composition complexation of reversible reaction |
| CN102992305A (en) * | 2012-10-25 | 2013-03-27 | 中南大学 | Graphene material and preparation method of solid graphene |
| CN102965189A (en) * | 2012-11-09 | 2013-03-13 | 天津耀宇生物技术有限公司 | Method for extracting chrysalis oil |
| CN102989416A (en) * | 2012-11-30 | 2013-03-27 | 中国农业科学院油料作物研究所 | Aflatoxin adsorbent and method for removing aflatoxins in edible vegetable oil |
| CN103540394A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for extracting silkworm pupa oil by utilizing ultrasonic assisted aqueous enzymatic method |
| CN103540402A (en) * | 2013-10-31 | 2014-01-29 | 西南大学 | Method for reducing content of cholesterol in chrysalis oil |
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