CN106560508A - Production method for Chinese prickly ash seed oil - Google Patents
Production method for Chinese prickly ash seed oil Download PDFInfo
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- CN106560508A CN106560508A CN201510636979.6A CN201510636979A CN106560508A CN 106560508 A CN106560508 A CN 106560508A CN 201510636979 A CN201510636979 A CN 201510636979A CN 106560508 A CN106560508 A CN 106560508A
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Abstract
The invention discloses a production method for Chinese prickly ash seed oil. The production method mainly comprises the following steps: subjecting Chinese prickly ash seeds to crushing, stir frying, oil pressing, de-waxing and extraction with a weakly polar organic solvent and separately treating upper extract and lower extract, wherein the upper extract undergoes recovery of the organic solvent and is then reused, and a concentrated substance is free fatty acid; and the lower extract is oil with a low acid value, and a conventional refining process is employed for low-temperature drying, decoloring and filtering of the oil so as to obtain qualified product oil with an acid value in a range prescribed in national standards in China. According to the invention, the coats and the kernels of the Chinese prickly ash seeds are subjected to oil pressing at the same time, so considerable alpha-linolenic acid in the kernels and considerable volatile oil in the coats are reserved in the obtained crude oil; the crude oil undergoes de-waxing at first and is then subjected to extraction with the organic solvent to extract most free fatty acid, and then alkali refining is carried out, so product yield is improved, and the added value of the byproducts consisting of wax and free fatty acid is high; and low-temperature refining process reduces loss of the volatile oil and oxidation of alpha-linolenic acid. The produced Chinese prickly ash seed oil contains more than 30% of alpha-linolenic acid and has rich spicy fragrance of Chinese prickly ash. The production method provided by the invention realizes comprehensive processing and utilization of the Chinese prickly ash seeds.
Description
Technical field
The present invention relates to the preparing technical field of edible oil, more particularly to a kind of production method of Fructus Zanthoxyli oil.
Background technology
The perennial shrub of Zanthoxylum Rutaceae or dungarunga, are one of eight traditional big flavorings of China.Wild pepper seed is the byproduct in the production of Chinese prickly ash pericarp, it was reported that China's annual output there are about more than 130 ten thousand tons.Wild pepper seed contains more than 20% crude fat, and wherein alpha-linolenic acid content contains substantial amounts of volatile essential oils more than 30%, in pepper seed skin, and Fructus Zanthoxyli oil is that one kind is of high nutritive value and characteristic flavored oils.But, because the acid number of Fructus Zanthoxyli oil is high and wax content is high so as to which the difficulty of processing and utilization is larger.The existing process technology of Fructus Zanthoxyli oil mainly has following several：(1) pepper seed skin is crushed together with benevolence, disposable Extractive crudeoil, then refines and become edible oil；(2) first pepper seed skin carried out into extraction, seed peel oil is used for iundustrial oil, then wild pepper seed benevolence is extracted, and refining is obtained edible oil；(3) first wild pepper seed peeled, then lixiviation process and oil extraction by pressing is respectively adopted to pepper seed skin and benevolence；(4) after wild pepper seed is crushed, supercritical CO is used2Extract to obtain edible oil.The subject matter that above-mentioned processing method is present：One is to use supercritical CO2The Fructus Zanthoxyli oil of extraction equipment production, quality is good but equipment investment is big, and production cost is high；Two is to produce Fructus Zanthoxyli oil with extraction method, and large-scale leaching equipment has that equipment investment is big, starving, and it is up to standard that small-sized leaching equipment has that precipitation is difficult to；Three is that wild pepper seed exfoliant effect is undesirable, and decortication cost is also higher；Four is that, using traditional alkali-refining deacidification method, refining consumption is too big, and product yield is low.
The content of the invention
For the deficiency that above-mentioned prior art is present, the present invention provides a kind of process is simple, low production cost, the production method of the comprehensive utilization Fructus Zanthoxyli oil that effect is good, added value is high.
A kind of production method of Fructus Zanthoxyli oil, comprises the technical steps that：
(1) particle of the mesh of 6 mesh -60 is broken into after is cleaned wild pepper seed；
(2) by broken particle under the conditions of 70 DEG C -130 DEG C, fry -30 minutes 10 minutes；
(3) the wild pepper seed particle fried is squeezed to obtain wild pepper seed crude oil；
(4) crude oil is carried out into conventional dewaxing, must dewax crude oil and wax；
(5) weakly polar organic solvent of 1 to 3 times of crude oil volume is added in dewaxing crude oil, is stirred under room temperature
20-60 minutes, then stand 30-60 minutes, obtain stratified liquid, wherein supernatant liquid be organic solvent with
The mixed liquor of free fatty, lower floor's liquid is the relatively low grease of acid value；
(6) supernatant liquid is taken out and is separated, organic solvent recycling, concentrate is free fatty；The grease of lower floor's liquid is refined again to obtain product oil.
The production method of described Fructus Zanthoxyli oil, it is characterised in that the described wild pepper seed particle size after cracking preferably mesh of 10 mesh -20.
The production method of described Fructus Zanthoxyli oil, it is characterised in that described preferably 100 DEG C -110 DEG C of wild pepper seed frying condition, frying -20 minutes 15 minutes.
The production method of described Fructus Zanthoxyli oil, it is characterised in that described weakly polar organic solvent, including methyl alcohol, ethanol, acetone, propyl alcohol or similar solvent.
The production method of described Fructus Zanthoxyli oil, it is characterized in that ethanol of the described weakly polar organic solvent preferred volume concentration for 70%-95%, and crude oil is 1: 2-2.5 with the volume ratio of the ethanol, preferably 20 DEG C -30 DEG C of extraction temperature, mixing time be 30-40 minutes, time of repose 40-60 minutes.
The production method of described Fructus Zanthoxyli oil, it is characterised in that described extractant ethanol preferred volume concentration is the ethanol of 90%-95%.
The production method of described Fructus Zanthoxyli oil, it is characterised in that described oil and fat refining adopts vacuum drying process, and vacuum drying process temperature is 60 DEG C -80 DEG C；Vacuum -0.07MPa--0.085Mpa；- 90 minutes 30 minutes drying time.
The production method of described Zanthoxylum essential oil, it is characterised in that the vacuum drying process condition preferable temperature is 75 DEG C -80 DEG C；Vacuum -0.075MPa--0.08Mpa；Drying time is -60 minutes 40 minutes.
The present invention compared with prior art, has an advantage in that (1) jointly extracts oil pepper seed skin with benevolence, and not only processing technology is simple, and a large amount of ethereal oils contained in a large amount of alpha-linolenic acids and skin contained in benevolence are remained in crude oil；(2) crude oil is dewaxed in advance, on the one hand dewaxing crude oil is conducive to the deacidifying process in later stage, reduces processing cost, and the added value of the wax on the other hand parsing is higher；(3) depickling is carried out in two steps, first extract the most of free fatties in dewaxing crude oil with ethanol, on the one hand the acid number for making crude oil is controlled in relatively low level, carry out beneficial to economical and practical alkali-refining deacidification, the refining techniques of more existing Fructus Zanthoxyli oil reduces refining consumption, product yield is improved, the free fatty concentrated after the extraction of another aspect ethanol is high compared with the added value of the byproduct soap stock that alkali refining is obtained；(4) in addition to frying seed and carrying out at 100 DEG C or so, all control is accomplished below at 80 DEG C for post-production process, reduces the loss of ethereal oil and the oxidation of alpha-linolenic acid.The Fructus Zanthoxyli oil produced with the method contains more than 30% alpha-linolenic acid, with the strong pungent fragrance of Chinese prickly ash, it is the oil of the edible flavouring rich in alpha-linolenic acid of great characteristic, its byproduct wax and free fatty can be used as chemical industry or the raw materials of biodiesel, the comprehensive processing and utilization that the present invention has preferably been carried out to wild pepper seed.
Specific embodiment
Embodiment 1
Weigh 20 kilograms of the wild pepper seed after cleaning, it is broken into more than 6 mesh, less than the particle of 60 mesh with pulverizer, in electric frying pan, 100 DEG C of constant temperature, frying 20 minutes is obtained 5.20 kilograms of the crude oil that acid number is 42mgkoH/100g with oil press, this crude oil is first warmed up to into 80 DEG C, dewax under 5-6 DEG C of environment again, must dewax 4.26 kilograms of crude oil, 0.94 kilogram of byproduct wax.4.26 kilograms of dewaxing crude oils are added (ethanol and the volume ratio of water are 70: 30 in the alcohol) in 12.78 kilogram 70% of edible alcohol；60 minutes (essence takes temperature and is typically not greater than 50 DEG C) is stirred at ambient temperature, then 60 minutes is stood, and forms upper and lower two-layer liquid phase.Upper liquid obtains 0.38 kilogram of free fatty concentrate by 12.2 kilograms of atmospheric evaporation recovered alcohol；Subnatant is grease, 3.88 kilograms of weight, acid number 4.7mgkoH/100g.Separate with depickling, soap stock according to a conventional method plus in alkali, water washing, then using vacuum drying method, be 80 DEG C, be dried 60 minutes under vacuum -0.07MPa in temperature, decolourize, obtain 3.67 kilograms of the product oil that acid number is 1.1mgkoH/100g.
Embodiment 2
Weigh 20 kilograms of the wild pepper seed after cleaning, it is broken into more than 10 mesh, less than the particle of 40 mesh with pulverizer, it is put into frying pan, the frying 15 minutes of 110 DEG C of constant temperature, 5.1 kilograms of the crude oil that acid number is 45.2mgkoH/100g is obtained with oil press, this crude oil is dewaxed under 5-6 DEG C of environment, must dewax 4.15 kilograms of crude oil, 0.95 kilogram of byproduct wax.4.15 kilograms of dewaxing crude oils are added in 10.37 kilograms of acetone, is stirred 20-30 minutes under 15 DEG C of room temperature conditions, then stand 40 minutes, form upper and lower two-layer liquid.Upper liquid reclaims 9.53 kilograms of acetone by atmospheric evaporation, obtains 0.41 kilogram of free fatty concentrate；Subnatant is 3.74 kilograms of the grease of acid number 12.2mgkoH/100g, separate with depickling, soap stock according to a conventional method plus in alkali, water washing, it is dried 40 minutes under 75 DEG C, vacuum -0.075MPa, decolourizes, obtains 3.59 kilograms of the product oil that acid number is 0.7mgkoH/100g.
Embodiment 3
After 20 kilograms of wild pepper seed are cleaned, it is broken into more than or equal to 10 mesh, less than the particle of 20 mesh with pulverizer, in pouring electric frying pan into, 130 DEG C of constant temperature is fried 10 minutes, 5.32 kilograms of the crude oil that acid number is 46.1mgkoH/100g is obtained with oil extruder, this crude oil is first warmed up to into 60 DEG C, then dewaxed under 4-5 DEG C of environment, must be dewaxed 4.34 kilograms of crude oil, 0.98 kilogram of byproduct wax.It is in 95% ethanol, to stir at 30 DEG C 40 minutes that 4.34 kilograms of dewaxing crude oil is added into 8.68 kilograms of volumetric concentrations, then stands 30 minutes, forms upper and lower two-layer liquid, separates to obtain upper and lower two-layer liquid.Upper liquid obtains 0.45 kilogram of free fatty concentrate by 8.42 kilograms of atmospheric evaporation recovered alcohol；Subnatant is 3.89 kilograms of the grease that acid number is 11.3mgkoH/100g, separate with depickling, soap stock according to a conventional method plus in alkali, water washing, it is dried 90 minutes under 60 DEG C, vacuum -0.085MPa, decolourizes, obtains 3.77 kilograms of the product oil that acid number is 1.0mgkoH/100g.
Embodiment 4
Weigh 20 kilograms of the wild pepper seed after cleaning, it is broken into more than 6 mesh, less than the particle of 40 mesh with pulverizer, in electric frying pan, 70 DEG C of constant temperature is fried 30 minutes, 5.11 kilograms of the crude oil that acid number is 35.7mgkoH/100g is obtained with oil press, this crude oil is dewaxed under 5-6 DEG C of environment, must dewax 4.24 kilograms of crude oil, 0.87 kilogram of byproduct wax.It is in 90% ethanol, to stir under 20 DEG C of normal temperature 50 minutes that 4.24 kilograms of dewaxing crude oils are added 10.6 kilograms of volumetric concentrations, then stands 60 minutes, forms upper and lower two-layer liquid, separates to obtain upper and lower two-layer liquid.Upper liquid obtains 0.41 kilogram of free fatty concentrate by 10.31 kilograms of atmospheric evaporation recovered alcohol；Subnatant is 3.83 kilograms of the grease that acid number is 12.8mgkoH/100g, separate with depickling, soap stock according to a conventional method plus in alkali, water washing, it is dried 30 minutes under 75 DEG C, vacuum -0.08MPa, decolourizes, obtains 3.73 kilograms of the product oil that acid number is 0.8mgkoH/100g.
Claims (8)
1. a kind of production method of Fructus Zanthoxyli oil, comprises the technical steps that：
(1) particle of the mesh of 6 mesh -60 is broken into after is cleaned wild pepper seed；
(2) by broken particle under the conditions of 70 DEG C -130 DEG C, fry -30 minutes 10 minutes；
(3) the wild pepper seed particle fried is squeezed to obtain wild pepper seed crude oil；
(4) crude oil is carried out into conventional dewaxing, must dewax crude oil and wax；
(5) weakly polar organic solvent of 1 to 3 times of crude oil volume is added in dewaxing crude oil, stir 20-60 minutes under room temperature, then stand 30-60 minutes, obtain stratified liquid, wherein supernatant liquid is the mixed liquor of organic solvent and free fatty, and lower floor's liquid is the relatively low grease of acid value；
(6) supernatant liquid is taken out and is separated, organic solvent recycling, concentrate is free fatty；The grease of lower floor's liquid is refined again to obtain product oil.
2. the production method of Fructus Zanthoxyli oil according to claim 1, it is characterised in that the described wild pepper seed particle size after cracking preferably mesh of 10 mesh -20.
3. the production method of Fructus Zanthoxyli oil according to claim 1, it is characterised in that described preferably 100 DEG C -110 DEG C of wild pepper seed frying condition, frying -20 minutes 15 minutes.
4. the production method of Fructus Zanthoxyli oil according to claim 1, it is characterised in that described weakly polar organic solvent, including methyl alcohol, ethanol, acetone, propyl alcohol or similar solvent.
5. the production method of Fructus Zanthoxyli oil according to claim 1, it is characterized in that ethanol of the described weakly polar organic solvent preferred volume concentration for 70%-95%, and crude oil is 1: 2-2.5 with the volume ratio of the ethanol, preferably 20 DEG C -30 DEG C of extraction temperature, mixing time be 30-40 minutes, time of repose 40-60 minutes.
6. the production method of the Fructus Zanthoxyli oil described in claim 5, it is characterised in that described extractant ethanol preferred volume concentration for 90%-95% ethanol.
7. the production method of the Fructus Zanthoxyli oil described in claim 1, it is characterised in that described oil and fat refining adopts vacuum drying process, and vacuum drying process temperature is 60 DEG C -80 DEG C；Vacuum -0.07MPa--0.085Mpa；- 90 minutes 30 minutes drying time.
8. the production method of Zanthoxylum essential oil according to claim 7, it is characterised in that the vacuum drying process condition preferable temperature is 75 DEG C -80 DEG C；Vacuum -0.075MPa--0.08Mpa；Drying time is -60 minutes 40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510636979.6A CN106560508A (en) | 2015-10-03 | 2015-10-03 | Production method for Chinese prickly ash seed oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510636979.6A CN106560508A (en) | 2015-10-03 | 2015-10-03 | Production method for Chinese prickly ash seed oil |
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| CN106560508A true CN106560508A (en) | 2017-04-12 |
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| CN201510636979.6A Withdrawn CN106560508A (en) | 2015-10-03 | 2015-10-03 | Production method for Chinese prickly ash seed oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801643A (en) * | 2019-11-19 | 2020-02-18 | 四川丁点儿食品开发股份有限公司 | Device and method for removing bitter taste of pepper extract |
| CN111205923A (en) * | 2020-01-13 | 2020-05-29 | 四川嘉威德农业科技有限公司 | Processing technology of pure zanthoxylum oil rich in linolenic acid |
-
2015
- 2015-10-03 CN CN201510636979.6A patent/CN106560508A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110801643A (en) * | 2019-11-19 | 2020-02-18 | 四川丁点儿食品开发股份有限公司 | Device and method for removing bitter taste of pepper extract |
| CN111205923A (en) * | 2020-01-13 | 2020-05-29 | 四川嘉威德农业科技有限公司 | Processing technology of pure zanthoxylum oil rich in linolenic acid |
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Application publication date: 20170412 |