CN105061192A - Method for extracting and preparing palmitic acid from waste porcellanite in corn fat processing - Google Patents
Method for extracting and preparing palmitic acid from waste porcellanite in corn fat processing Download PDFInfo
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- CN105061192A CN105061192A CN201510438713.0A CN201510438713A CN105061192A CN 105061192 A CN105061192 A CN 105061192A CN 201510438713 A CN201510438713 A CN 201510438713A CN 105061192 A CN105061192 A CN 105061192A
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Abstract
The invention discloses a method for extracting and preparing palmitic acid from waste porcellanite in corn fat processing. The method comprises the following steps: (1) extracting and filtering waste porcellanite by using petroleum ether, and evaporating petroleum ether to obtain coarse wax; (2) adding ethanol into the coarse wax, wherein the addition ratio of coarse wax and ethanol is 1g: (5-15) ml, heating and dissolving the mixture, uniformly shaking the mixture and cooling the mixture to room temperature, precipitating the mixture for 0.5-1.5 hours, separating the precipitate and drying the precipitate to obtain refined wax; (3) adding an ethanol solution of KOH into the refined wax, heating the mixture to be boiled, carrying out reflux for 1-1.5 hours, stopping reflux, adding water, uniformly mixing the mixture, then adding ether, uniformly mixing the mixture, and leaving the mixture to stand to layer so as to obtain a lower layer aqueous solution; and (4) adding an HCl solution into the lower layer aqueous solution, uniformly mixing the mixture, then adding ether, uniformly mixing the mixture, and leaving the mixture to stand to layer to obtain an ether layer, and drying the ether layer to obtain palmitic acid. According to the method disclosed by the invention, palmitic acid is extracted and obtained from waste porcellanite in a fat processing process for the first time, and the extraction method is simple, can be used for realizing recycle of wastes, and has relatively high economical and environmental-friendly benefits.
Description
Technical field
The present invention relates to a kind of extraction from the useless white bole of corn fats and oils processing and prepare the method for palmitinic acid.
Background technology
Palmitinic acid (Palmiticacid), also known as Palmiticacid, is a kind of saturated higher fatty acid, is widespread in nature, and all contains the Palmiticacid component that content does not wait in nearly all grease.In the Chinese vegetable tallow of China's special product, the content of Palmiticacid can up to more than 60%, and in the plam oil of palm tree fruit, content is approximately 40%, content very low (if the content in rapeseed oil is then less than 2%) in some greases.After Chinese vegetable tallow or Hydrolysis of Palm Oil, fractionation, expression separation unsaturated fatty acids, through recrystallization i.e. obtained palmitinic acid.
Palmitinic acid is of many uses, can be used as precipitation agent, chemical reagent (as analytical standard material), water-resisting agent, defoamer, manufacture the raw material of other foodstuff additive as glycerin fatty acid ester, lipid acid sorbitan ester, sugar ester etc., also can be used as spices batching, produce the raw material of candle, soap, lubricating grease, tenderizer and synthetic detergent.Palmitinic acid is for the manufacture of Syntomycini Palmitas and various palmitinic acid metal-salt, and its sodium salt or sylvite can be used as emulsifying agent during letex polymerization, and aluminium salt and zinc salt etc. are in lubricant, coating, glossy black and softening agent.These product have special aroma and flavour, by national regulation, can be used for preparing various flavouring agent, are also used as the raw material of defoamer and other foodstuff additive.
Useless white bole is as a kind of tankage produced in corn course of oil processing, less for its research at present, how directly to abandon as waste.If therefrom can prepare palmitinic acid by extraction and isolation, and develop it, its economic benefit, social benefit can be very remarkable, have wide DEVELOPMENT PROSPECT.
Summary of the invention
For above-mentioned prior art, the object of this invention is to provide a kind of extraction from the useless white bole of corn fats and oils processing and prepare the method for palmitinic acid.
For achieving the above object, the present invention adopts following technical proposals:
From the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid, step is as follows:
(1) the useless white bole after being used in the course of processing by corn grease adopts sherwood oil to extract, and filters, and steams except sherwood oil, obtains waxy stone;
(2) in the obtained waxy stone of step (1), add ethanol, the ratio of waxy stone and amount of alcohol added is 1g:(5-15) ml, heating for dissolving, be cooled to room temperature after shaking up, adularescent material is separated out, precipitation 0.5-1.5h, isolate precipitation, dry, obtain smart wax;
(3) in the obtained smart wax of step (2), add the ethanolic soln of KOH, be heated to boiling, backflow 1-1.5h, after stopping backflow, adds water wherein, mixing, then adds ether, and mixing, stratification, obtains lower aqueous solution.The ratio of the add-on of essence wax, the ethanolic soln of KOH, water and ether is 1g:(12-13) ml:(12-13) ml:25ml;
(4) in lower aqueous solution, add HCl solution, mixing, then add ether, mixing, stratification, obtains ether layer, dry, obtains palmitinic acid.
In step (1), the add-on of sherwood oil is useless kaolinic 2-4 times of quality volume (amount namely adding sherwood oil in every gram of useless white bole is 2-4mL); Preferably, the add-on of sherwood oil is useless kaolinic 3 times of quality volumes.
In step (1), adding the number of times that sherwood oil carries out extracting is 2-4 time, extracts 0.5-2.5h at every turn.
In step (2), the temperature of heating for dissolving is 75-95 DEG C.
In step (2), precipitation separation adopts centrifuging, and centrifugal rotational speed is 2000 ~ 10000r/min, and centrifugation time is 3 ~ 8min.
In step (3), the concentration of the ethanolic soln of described KOH is 26-30g/L.The ethanolic soln object adding KOH is for saponification, and the concentration of the ethanolic soln of KOH is too low, then saponification time is long, and saponification is incomplete; The excessive concentration of the ethanolic soln of KOH, then target compound easily decomposes.
In step (4), the mass concentration of described HCl solution is 50%.The object adding HCl solution be in and alkali lye, make the pH=7 of solution or below 7, under sour environment, target product palmitinic acid solubleness is low, easily separates.
In step (4), the ratio of the add-on of the smart wax of HCl solution, ether and step (2) is (16-18) ml:25ml:1g.
In the present invention, the room temperature of indication refers to 15-30 DEG C.
After the sample prepared the present invention carries out esterification process, be detected as Uniphat A60 through GC-MS, illustrate that the sample of preparation is palmitinic acid.
Beneficial effect of the present invention:
(1) extract in the useless white bole that system of the present invention produces first from course of oil processing and obtain palmitinic acid, extracting method is simple, can realize the recycling of refuse, have higher economy and environmental benefit.
(2) the useless white bole after adopting method of the present invention to extract palmitinic acid, can be reused for the machining process of grease.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1: the extraction preparation of palmitinic acid in useless white bole
Take useless white bole 100g, add 300ml sherwood oil, stirred at ambient temperature extracts 1.5h, filters, and extracts 3 times under similarity condition, is merged by filtering solution, steams and desolventizes to obtain faint yellow waxy stone.In waxy stone, add 25ml dehydrated alcohol, 90 DEG C of heating in water bath, to all dissolving, are cooled to room temperature after shaking up, and adularescent material is separated out, after precipitation 1h, under 6000RPM condition, centrifugal 5min, abandons supernatant, repeat 8 times, white precipitate is volatilized, through weighing final white smart wax 1.89g.Taking white smart wax 0.2g is dissolved in 2ml sherwood oil, its main component of infrared spectroscopy analyzing and testing, infrared spectra testing conditions: resolving power is 4cm
-1, diaphragm is set to 6mm, sweep velocity 7.5KHz, and test specification is 500 ~ 4000cm
-1.Smart wax main component is iso-octyl palmitate after testing.
Get 1g iso-octyl palmitate, add 28.05g/LKOH solution 12.5ml, boiling reflux 1h.Add distilled water 12.5ml wherein after stopping backflow, mixing, then add ether 25ml, mixing, static layering, obtains lower floor's solution.Under rocking, 17ml50% (mass concentration) HCl solution is added in lower floor's solution.In this solution, add ether 25ml again, mixing, layering, obtains ether layer, revolves evaporate to dryness dry, obtains sample (palmitinic acid) 0.65g.
Prepare the H of 7% concentration
2sO
4the each 0.5ml of methanol solution, in 2ml centrifuge tube, takes sample 5mg and joins the H prepared
2sO
4in methanol solution, 65 DEG C of Water Under bath heating 20min, add 1ml normal hexane, vibration mixing 1min after cooling, static 6min, draw supernatant (normal hexane layer) in 2ml centrifuge tube with liquid-transfering gun, ventilating kitchen normal temperature volatilization about 10h, obtains sample concentration liquid, 4 DEG C of refrigerator and cooled are hidden and are preserved, GC-MS detects confirmation, is be Uniphat A60, and what show preparation is palmitinic acid.
Embodiment 2: the extraction preparation of palmitinic acid in useless white bole
Take useless white bole 100g, add 200ml sherwood oil, stirred at ambient temperature extracts 0.5h, filters, and extracts 2 times under similarity condition, is merged by filtering solution, steams and desolventizes to obtain faint yellow waxy stone.In waxy stone, add 12ml dehydrated alcohol, 75 DEG C of heating in water bath, to all dissolving, are cooled to room temperature after shaking up, and adularescent material is separated out, and after precipitation 0.5h, centrifugal 3min under 10000RPM condition, abandons supernatant, repeat 5 times, volatilized by white precipitate.Through weighing final white smart wax 1.84g, its main component of infrared spectroscopy analyzing and testing is palmitinic acid isooctyl, and testing conditions is with embodiment 1.
Get 3g iso-octyl palmitate, add 28.05g/LKOH38ml, boiling reflux 1.5h, stop backflow, add distilled water 38ml wherein, mixing.Add ether 76ml again, mixing, static layering, obtains lower floor's solution.Rock down in lower floor's solution and add 51ml50%HCl solution, then add ether 76ml in this solution, mixing layering, obtains ether layer, revolves evaporate to dryness dry, obtain sample (palmitinic acid) 2g.
The detection method of sample is with embodiment 1.
Embodiment 3: the extraction preparation of palmitinic acid in useless white bole
Take useless white bole 100g, add 400ml sherwood oil, stirred at ambient temperature extracts 2.5h, filters, and extracts 4 times under similarity condition, is merged by filtering solution, steams and desolventizes to obtain waxy stone.In waxy stone, add 35ml dehydrated alcohol, 95 DEG C of heating in water bath, to all dissolving, are cooled to room temperature after shaking up, and adularescent material is separated out, and after precipitation 1.5h, centrifugal 8min under 2000RPM condition, abandons supernatant, repeat 10 times, volatilized by white precipitate.Weigh final smart wax 1.85g, and its main component of infrared spectroscopy analyzing and testing is palmitinic acid isooctyl, and testing conditions is with embodiment 1.
Get iso-octyl palmitate 5g, add 28.05g/LKOH62.5ml, boiling reflux 1.5h, stop backflow, add distilled water 62.5ml wherein, mixing.In this liquid, add ether 150ml, mixing, static layering, obtains lower floor's solution.In lower floor's solution, add 85ml50%HCl solution under rocking, then add ether 150ml in this liquid, mixing layering, obtains ether, revolves evaporate to dryness dry, obtain sample (palmitinic acid) 3.1g.
The detection method of sample is with embodiment 1.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid, it is characterized in that, step is as follows:
(1) the useless white bole after being used in the course of processing by corn grease adopts sherwood oil to extract, and filters, and steams except sherwood oil, obtains waxy stone;
(2) in the obtained waxy stone of step (1), add ethanol, the ratio of waxy stone and amount of alcohol added is 1g:(5-15) ml, heating for dissolving, be cooled to room temperature after shaking up, adularescent material is separated out, precipitation 0.5-1.5h, isolate precipitation, dry, obtain smart wax;
(3) in the obtained smart wax of step (2), add the ethanolic soln of KOH, be heated to boiling, backflow 1-1.5h, after stopping backflow, adds water wherein, mixing, add ether again, mixing, stratification, lower aqueous solution, the ratio of the add-on of the ethanolic soln of smart wax, KOH, water and ether is 1g:(12-13) ml:(12-13) ml:25ml;
(4) in lower aqueous solution, add HCl solution, mixing, then add ether, mixing, stratification, obtains ether layer, dry, obtains palmitinic acid.
2. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (1), the add-on of sherwood oil is useless kaolinic 2-4 times of quality volume.
3. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 2, it is characterized in that, in step (1), the add-on of sherwood oil is useless kaolinic 3 times of quality volumes.
4. as claimed in claim 1 from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid, it is characterized in that, in step (1), adding the number of times that sherwood oil carries out extracting is 2-4 time, extracts 0.5-2.5h at every turn.
5. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (2), the temperature of heating for dissolving is 75-95 DEG C.
6. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (2), precipitation separation adopts centrifuging, centrifugal rotational speed is 2000 ~ 10000r/min, and centrifugation time is 3 ~ 8min.
7. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (3), the concentration of the ethanolic soln of described KOH is 26-30g/L.
8. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (4), the mass concentration of described HCl solution is 50%.
9. from the useless white bole of corn fats and oils processing, extract the method preparing palmitinic acid as claimed in claim 1, it is characterized in that, in step (4), the ratio of the add-on of the smart wax of HCl solution, ether and step (2) is (16-18) ml:25ml:1g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438713.0A CN105061192B (en) | 2015-07-23 | 2015-07-23 | The method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing |
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| CN201510438713.0A CN105061192B (en) | 2015-07-23 | 2015-07-23 | The method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing |
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| CN105061192B CN105061192B (en) | 2016-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108569963A (en) * | 2018-05-02 | 2018-09-25 | 广东广益科技实业有限公司 | A kind of production technology of palmitic acid waste residue recycling |
Citations (2)
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| CN103940654A (en) * | 2014-05-06 | 2014-07-23 | 山东师范大学 | Method for extracting vitamin E from waste kaolin and thin layer chromatography detection method |
| CN104761445A (en) * | 2015-01-09 | 2015-07-08 | 内蒙古大学 | Method for extracting chemical components from root of mongolian medicine Cymbaria dahurica |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103940654A (en) * | 2014-05-06 | 2014-07-23 | 山东师范大学 | Method for extracting vitamin E from waste kaolin and thin layer chromatography detection method |
| CN104761445A (en) * | 2015-01-09 | 2015-07-08 | 内蒙古大学 | Method for extracting chemical components from root of mongolian medicine Cymbaria dahurica |
Non-Patent Citations (3)
| Title |
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| SIMON J.T. POLLARD ET AL.: "《THE REUSE OF SPENT BLEACHING EARTH: A FEASIBILITY STUDY IN WASTE MINIMISATION FOR THE EDIBLE OIL INDUSTRY》", 《BIORESOURCE TECHNOLOGY》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108569963A (en) * | 2018-05-02 | 2018-09-25 | 广东广益科技实业有限公司 | A kind of production technology of palmitic acid waste residue recycling |
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