CN105061192B - The method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing - Google Patents
The method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing Download PDFInfo
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- CN105061192B CN105061192B CN201510438713.0A CN201510438713A CN105061192B CN 105061192 B CN105061192 B CN 105061192B CN 201510438713 A CN201510438713 A CN 201510438713A CN 105061192 B CN105061192 B CN 105061192B
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a kind of method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing, step is as follows: useless kaolin employing petroleum ether is extracted by (1), filters, petroleum ether is evaporated off, obtains waxy stone；(2) adding ethanol in waxy stone, the ratio of waxy stone and amount of alcohol added is 1g:(5 15) ml, heating for dissolving, it is cooled to room temperature after shaking up, precipitates 0.5 1.5h, isolate precipitation, be dried, obtain fine wax；(3) adding the ethanol solution of KOH in fine wax, be heated to boiling, reflux 1 1.5h, after stopping backflow, adds water, mixing, adds ether, mixing, and stratification obtains lower aqueous solution；(4) in lower aqueous solution, add HCl solution, mixing, add ether, mixing, stratification, obtain ether layer, be dried, obtain Palmic acid.Extracting in the useless kaolin that system of the present invention produces first from course of oil processing and obtain Palmic acid, extracting method is simple, can realize the recycling of refuse, have higher economical and environmentally friendly benefit.
Description
Technical field
The present invention relates to a kind of method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing.
Background technology
Palmic acid (Palmitic acid), also known as palmitic acid, is a kind of saturated higher fatty acid, is widespread in nature,
Almost all of oils and fats all contains the palmitic acid component that content does not waits.In the Chinese tallow of China's special product, the content of palmitic acid can be high
Reaching more than 60%, in the Petiolus Trachycarpi oil of palm fruit, content is about 40%, and in some oils and fatss, content is the lowest (such as Oleum Brassicae campestris
In content then less than 2%).After Chinese tallow or Hydrolysis of Palm Oil, fractional distillation, expression separation unsaturated fatty acid, through recrystallization
I.e. prepare Palmic acid.
Palmic acid is of many uses, can be used as precipitant, chemical reagent (as analytical standard material), waterproofing agent, froth breaking
Agent, manufactures the raw material such as fatty glyceride of other food additive, fatty acid sorbitan ester, sugar ester etc., can act also as
Spice dispensing, produces wax candle, soap, grease, softening agent and the raw material of synthetic detergent.Palmic acid is used for manufacturing tasteless chlorine
Mycin and various Palmic acid slaine, its sodium salt or potassium salt can be used as emulsion polymerization time emulsifying agent, aluminium salt and zinc salt etc. are used for moistening
In lubrication prescription, coating, glossy black and plasticizer.These product have special aroma and flavour, by national regulation, can be used for preparing various food
With spice, also serve as the raw material of defoamer and other food additive.
Useless kaolin is as a kind of leftover bits and pieces produced in Semen Maydis course of oil processing, less for its research at present, many as useless
Gurry directly abandons.If separation can therefrom be extracted prepare Palmic acid, and it is developed, its economic benefit, social benefit
Can be very notable, there is wide DEVELOPMENT PROSPECT.
Summary of the invention
For above-mentioned prior art, it is an object of the invention to provide a kind of extraction from the useless kaolin of Semen Maydis fats and oils processing and prepare palm fibre
The method of palmitic acid acid.
For achieving the above object, the present invention uses following technical proposals:
A kind of method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing, step is as follows:
(1) the useless kaolin after being used in the course of processing by Semen Maydis oils and fats uses petroleum ether to extract, and filters, oil is evaporated off
Ether, obtains waxy stone；
(2) adding ethanol in the waxy stone that step (1) prepares, the ratio of waxy stone and amount of alcohol added is 1g:(5-15) ml,
Heating for dissolving, is cooled to room temperature after shaking up, have whiteness to separate out, and precipitates 0.5-1.5h, isolates precipitation, is dried, obtains fine wax；
(3) adding the ethanol solution of KOH in the fine wax that step (2) prepares, be heated to boiling, reflux 1-1.5h, stops
After backflow, it is added thereto to water, mixing, add ether, mixing, stratification, obtain lower aqueous solution.Fine wax, KOH
The ratio of addition of ethanol solution, water and ether be 1g:(12-13) ml:(12-13) ml:25ml；
(4) in lower aqueous solution, add HCl solution, mixing, add ether, mixing, stratification, obtain ether layer,
It is dried, obtains Palmic acid.
In step (1), the addition of petroleum ether (adds stone for useless kaolinic 2-4 times of quality volume in i.e. every gram useless kaolin
The amount of oil ether is 2-4mL)；Preferably, the addition of petroleum ether is useless kaolinic 3 times of quality volumes.
In step (1), the number of times that addition petroleum ether carries out extracting is 2-4 time, extracts 0.5-2.5h every time.
In step (2), the temperature of heating for dissolving is 75-95 DEG C.
In step (2), precipitation separation uses centrifuging, and centrifugal rotational speed is 2000～10000r/min, and centrifugation time is 3～8min.
In step (3), the concentration of the ethanol solution of described KOH is 26-30g/L.Add KOH ethanol solution purpose be for
Saponification, the concentration of the ethanol solution of KOH is too low, then saponification time is long, and saponification is incomplete；The concentration mistake of the ethanol solution of KOH
Height, then object is susceptible to decompose.
In step (4), the mass concentration of described HCl solution is 50%.The purpose adding HCl solution is to neutralize alkali liquor, makes molten
The pH=7 of liquid or below 7, under sour environment, target product Palmic acid dissolubility is low, can be easily separated out.
In step (4), HCl solution, ether are (16-18) ml:25ml with the ratio of the addition of the fine wax of step (2):
1g。
In the present invention, the room temperature of indication refers to 15-30 DEG C.
After the sample preparing the present invention carries out esterification process, it is detected as methyl hexadecanoate through GC-MS, the sample of preparation is described
Product are Palmic acids.
Beneficial effects of the present invention:
(1) in the useless kaolin that system of the present invention produces first from course of oil processing, extraction obtains Palmic acid, and extracting method is simple,
The recycling of refuse can be realized, there is higher economical and environmentally friendly benefit.
(2) method using the present invention extracts the useless kaolin after Palmic acid, can be reused for the machining process of oils and fats.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, it should explanation, and the description below is merely to explain this
Bright, its content is not defined.
Embodiment 1: in useless kaolin prepared by the extraction of Palmic acid
Weighing useless kaolin 100g, add 300ml petroleum ether, under room temperature, 1.5h is extracted in stirring, filters, and extracts under similarity condition
3 times, filtering solution is merged, solvent is evaporated off and obtains faint yellow waxy stone.Adding 25ml dehydrated alcohol in waxy stone, 90 DEG C of water-baths add
Heat, to all dissolving, is cooled to room temperature, has whiteness to separate out after shaking up, after precipitation 1h, and centrifugal 5min under the conditions of 6000RPM,
Abandon supernatant, be repeated 8 times, white precipitate is volatilized, through weighing final white fine wax 1.89g.Weigh white fine wax 0.2g molten
In 2ml petroleum ether, infrared spectrometry analysis detects its main component, infrared spectrum testing conditions: resolution is 4cm-1,
Diaphragm is set to 6mm, scanning speed 7.5KHz, and test scope is 500～4000cm-1.Fine wax is mainly composed of palm fibre after testing
The palmitic acid different monooctyl ester of acid.
Take 1g iso-octyl palmitate, add 28.05g/L KOH solution 12.5ml, boiling reflux 1h.Stop backflow backward its
Middle addition distilled water 12.5ml, mixing, add ether 25ml, mixing, static layering, obtain lower floor's solution.Molten to lower floor
Liquid is rocking lower addition 17ml 50% (mass concentration) HCl solution.In this solution, add ether 25ml again, mix,
Layering, obtains ether layer, and rotation is evaporated dry, obtains sample (Palmic acid) 0.65g.
Prepare the H of 7% concentration2SO4Methanol solution each 0.5ml, in 2ml centrifuge tube, weighs sample 5mg and joins and prepare
H2SO4In methanol solution, heating in water bath 20min under the conditions of 65 DEG C, add 1ml normal hexane after cooling, vibration mixes 1min, quiet
Only 6min, draws supernatant (normal hexane layer) in 2ml centrifuge tube with liquid-transfering gun, and ventilating kitchen room temperature volatilization about 10h obtains sample
Product concentrated solution, stored refrigerated in 4 DEG C of refrigerators, GC-MS detects confirmation, is for methyl hexadecanoate, and show preparation is Palmic acid.
Embodiment 2: in useless kaolin prepared by the extraction of Palmic acid
Weighing useless kaolin 100g, add 200ml petroleum ether, under room temperature, 0.5h is extracted in stirring, filters, and extracts under similarity condition
2 times, filtering solution is merged, solvent is evaporated off and obtains faint yellow waxy stone.Adding 12ml dehydrated alcohol in waxy stone, 75 DEG C of water-baths add
Heat, to all dissolving, is cooled to room temperature, has whiteness to separate out after shaking up, be centrifuged 3 after precipitation 0.5h under the conditions of 10000RPM
Min, abandons supernatant, is repeated 5 times, and is volatilized by white precipitate.Through weighing final white fine wax 1.84g, infrared spectrometry analysis
Detecting it and be mainly composed of Palmic acid isooctyl, testing conditions is with embodiment 1.
Take 3g iso-octyl palmitate, add 28.05g/L KOH 38ml, boiling reflux 1.5h, stop backflow, add wherein
Enter distilled water 38ml, mixing.Add ether 76ml, mixing, static layering, obtain lower floor's solution.Shake in lower floor's solution
The dynamic lower 51ml 50%HCl solution that adds, then in this solution, add ether 76ml, mixing layering, obtain ether layer, rotation is evaporated
Dry, obtain sample (Palmic acid) 2g.
The detection method of sample is with embodiment 1.
Embodiment 3: in useless kaolin prepared by the extraction of Palmic acid
Weighing useless kaolin 100g, add 400ml petroleum ether, under room temperature, 2.5h is extracted in stirring, filters, and extracts under similarity condition
4 times, filtering solution is merged, solvent is evaporated off and obtains waxy stone.Adding 35ml dehydrated alcohol in waxy stone, 95 DEG C of heating in water bath are to entirely
Portion dissolves, and is cooled to room temperature, has whiteness to separate out after shaking up, centrifugal 8min under the conditions of 2000RPM after precipitation 1.5h,
Abandon supernatant, be repeated 10 times, white precipitate is volatilized.Weigh final fine wax 1.85g, and it is main that infrared spectrometry analysis detects it
Wanting composition is Palmic acid isooctyl, and testing conditions is with embodiment 1.
Take iso-octyl palmitate 5g, add 28.05g/L KOH 62.5ml, boiling reflux 1.5h, stop backflow, add wherein
Enter distilled water 62.5ml, mixing.In this liquid, add ether 150ml, mixing, static layering, obtain lower floor's solution.To
Lower floor's solution rocks lower addition 85ml 50%HCl solution, then in this liquid, adds ether 150ml, mixing layering,
Obtaining ether, rotation is evaporated dry, obtains sample (Palmic acid) 3.1g.
The detection method of sample is with embodiment 1.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention being not restricted to the described embodiments,
The change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify, all should
For equivalence substitute mode, within being included in protection scope of the present invention.
Claims (8)
1. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing, it is characterised in that step is as follows:
(1) the useless kaolin after being used in the course of processing by Semen Maydis oils and fats uses petroleum ether to extract, and filters, oil is evaporated off
Ether, obtains waxy stone；
(2) adding ethanol in the waxy stone that step (1) prepares, the ratio of waxy stone and amount of alcohol added is 1g:(5-15) ml, add
Heat of solution, is cooled to room temperature after shaking up, have whiteness to separate out, and precipitates 0.5-1.5h, isolates precipitation, is dried, obtains fine wax；
(3) adding the ethanol solution of KOH in the fine wax that step (2) prepares, be heated to boiling, reflux 1-1.5h, stops
After backflow, it is added thereto to water, mixing, add ether, mixing, stratification, obtain lower aqueous solution, fine wax, KOH
The ratio of addition of ethanol solution, water and ether be 1g:(12-13) ml:(12-13) ml:25ml；
(4) in lower aqueous solution, add HCl solution, mixing, add ether, mixing, stratification, obtain ether layer,
It is dried, obtains Palmic acid.
2. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (1), petroleum ether is (2-4) ml:1g with the ratio of useless kaolinic addition.
3. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 2, its feature exists
In, in step (1), petroleum ether is 3ml:1g with the ratio of useless kaolinic addition.
4. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (1), the number of times that addition petroleum ether carries out extracting is 2-4 time, extracts 0.5-2.5h every time.
5. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (2), the temperature of heating for dissolving is 75-95 DEG C.
6. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (2), precipitation separation uses centrifuging, and centrifugal rotational speed is 2000～10000r/min, and centrifugation time is 3～8min.
7. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (3), the concentration of the ethanol solution of described KOH is 26-30g/L.
8. the method that Palmic acid is prepared in extraction from the useless kaolin of Semen Maydis fats and oils processing as claimed in claim 1, its feature exists
In, in step (4), HCl solution, ether are (16-18) ml:25ml with the ratio of the addition of the fine wax of step (2):
1g。
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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 |
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| 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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| 《THE REUSE OF SPENT BLEACHING EARTH: A FEASIBILITY STUDY IN WASTE MINIMISATION FOR THE EDIBLE OIL INDUSTRY》;Simon J.T. Pollard et al.;《Bioresource Technology》;19931231;第45卷(第1期);53-58 * |
| 《废白土中回收油脂的研究与应用》;罗天发等;《粮油加工与食品机械》;20041231(第6期);44-46 * |
| 《改良水剂法对脱色废白土中油脂回收效果的研究》;罗鹏等;《农业机械》;20121231(第6期);49-51 * |
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