CN105837430A - Method for extracting linoleic acid from idesia polycarpa crude oil - Google Patents
Method for extracting linoleic acid from idesia polycarpa crude oil Download PDFInfo
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- CN105837430A CN105837430A CN201610284304.4A CN201610284304A CN105837430A CN 105837430 A CN105837430 A CN 105837430A CN 201610284304 A CN201610284304 A CN 201610284304A CN 105837430 A CN105837430 A CN 105837430A
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- Prior art keywords
- crude oil
- radix seu
- linoleic
- seu cortex
- linoleic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- 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
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting linoleic acid from idesia polycarpa crude oil and relates to the field of deep processing of agricultural products .The method mainly solves the problems that in the prior art, the technology for extracting linoleic acid from idesia polycarpa is complex, energy consumption is high, and linoleic acid is low in purity .The technology includes the following steps that firstly, the idesia polycarpa crude oil is filtered and degummed through a filtering thin film to obtain degummed oil; secondly, in the inert gas environment, sodium hydroxide or potassium hydroxide is added into the degummed oil, saponification is conducted, and acidification, washing and dehydration are conducted to obtain mixed fatty acid, wherein the mass fraction of sodium hydroxide or potassium hydroxide is 10-30%; thirdly, the mixed fatty acid is frozen and preprocessed; fourthly, an organic solvent is added, and linoleic acid is extracted through the freezing separation method.
Description
Technical field
The present invention relates to crop products polish field, is specifically that one is extracted linoleic from Radix seu Cortex Malloti nepalensis crude oil
Method.
Background technology
Linoleic acid is the fatty acid of needed by human, is the important substance sustained life, but can not synthesize in human body, it is necessary to from
Food absorbs.In human body, linoleic acid can be metabolized to arachidonic acid, it is possible to decrease the cholesterol in blood, reduces coronary heart disease
Occur.It addition, linoleic acid can be metabolized to eicosapentaenoic acid (EPA) and docosahexenoic acid (DHA) further, promote
Enter health.
Linoleic acid can be by extracting from plant and animal, and wherein Radix seu Cortex Malloti nepalensis seed is that China's extraction is linoleic important
Source, on the one hand, Radix seu Cortex Malloti nepalensis has that widely distributed, less demanding to soil, weather etc., adaptability is relatively strong, is suitable for ground quality,
Barren hill, beach, mountain planting, easily cultivate, easily promote；On the other hand, the content of Radix seu Cortex Malloti nepalensis Linoleic acid is higher, according to statistics on mountain
The content of seeds of a tung oil tree crude oil Linoleic acid can reach more than 80%.
From Radix seu Cortex Malloti nepalensis seed, extract linoleic technique at present be predominantly acidified degumming, saponification and pass through urea adduct method
Extract, but its problem that there is the following aspects:
One, cost height, complex process.To use the degumming agents such as substantial amounts of phosphoric acid, citric acid in acidifying degumming, cost is high, work
Skill is complicated；
Two, energy expenditure is big, product purity is low；
Three, reaction environment complexity, reaction process are difficult to control to.
Summary of the invention
It is an object of the invention to: for the problem of above-mentioned existence, it is provided that a kind of extraction linoleic acid from Radix seu Cortex Malloti nepalensis crude oil
Method, use the linoleic refining technique such as membrane filtration degumming, centrifugation, solve that cost in prior art is high, technique
The problems such as complexity, energy expenditure are big, product purity is the highest.
The technical solution used in the present invention is as follows:
The invention discloses one from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, comprise the following steps:
(1) Radix seu Cortex Malloti nepalensis crude oil passes through membrane filtration degumming, obtains degummed oil
(2) in the environment of noble gas, add sodium hydroxide or potassium hydroxide to degummed oil, carry out saponification and go forward side by side
Row is acidified, washes, is dehydrated and obtains fatty acid mixed, and wherein the weight fraction of sodium hydroxide or potassium hydroxide is 10%-30%；
(3) fatty acid mixed is carried out freezing pretreatment；
(4) add organic solvent, extract linoleic acid by freeze and separate method.
Further, concretely comprising the following steps of described step 1 membrane filtration degumming: moisten film surface with acetone solvent, to crude oil
Middle addition quality be quality of crude oil be the deionized water of 10%-20%, at 10～30 DEG C, pressure 100～400kPa, by crude oil with stream
Speed 0.2～0.8m3/h passes through thin film.
Further, described step 3 pretreatment concrete operations are: by fatty acid mixed under the temperature range of 2 DEG C-4 DEG C
Freezing 2-10 hour, rapid sucking filtration after taking-up.
As preferably, the organic solvent of described step 4 is the one of methanol, petroleum ether, acetone, normal hexane.
As preferably, the concentration of described methanol is at 85-95%.
As preferably, the concentration of described acetone is at least 85%.
Further, the freeze and separate method of described step 4 concretely comprises the following steps: 0 DEG C ,-5 ,-10 ,-20 ,-30 ,-40 difference
Freezing 0.5-1.5 hour, by filter type, crystal is separated, oil suction fibre adsorbs, the product after absorption, at-5-5 DEG C
Under be centrifuged separate, obtain high-purity linoleic acid.
As preferentially, described filtration membrane is by acetate fiber, polyurethane resin, the one of polyacrylate resin.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
One, the linoleic technique of extraction that the present invention provides is divided into membrane filtration degumming, saponification, separation and culture, separation, technique letter
Single, the principle of use is few, is difficult in the product be mixed into magazine, improves linoleic quality；
Two, use membrane filtration degumming to separate, on the one hand can simplify refinery practice.Ultrafiltration degumming can replace traditional aquation and take off
Glue and two operations of alkali refining, reduce energy expenditure simultaneously, be substantially reduced production cost.On the other hand, reduce waste discharge, due to
Not having acidified, alkali refining operation, wastewater discharge declines in a large number；
Three, by freezing pretreatment and freeze and separate, according to linoleic acid with other satisfied fatty acid, impurity etc. at organic solvent
The difference of middle dissolubility and linoleic acid is proposed, its linoleic purity extracted can reach more than 90%.
Detailed description of the invention
The present invention is described in detail below.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Specific embodiment 1: present embodiment discloses one and extract linoleic method from Radix seu Cortex Malloti nepalensis crude oil, its feature exists
In, comprise the following steps:
(1) moisten filtration membrane surface with acetone solvent, in crude oil add quality be quality of crude oil be the deionized water of 10%,
At 10 DEG C, pressure 100kPa, by crude oil with flow velocity 0.2m3/h by filtration membrane, described filtration membrane is by acetate fiber
Make.
(2) in the environment of noble gas, add sodium hydroxide to degummed oil, carry out saponification carrying out be acidified, water
Washing, be dehydrated and obtain fatty acid mixed, wherein the weight fraction of sodium hydroxide is 10%；
(3) by fatty acid mixed freezing 2 hours, rapid sucking filtration after taking-up under the temperature range of about 2 DEG C；
(4) adding organic solvent methanol, extract linoleic acid by freeze and separate method, freeze and separate method concretely comprises the following steps: 0
DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 0.5 hour respectively, by filter type, crystal is separated, inhale with oil suction fibre
Attached, after absorption product, is centrifuged separating at-5 DEG C, obtains high-purity linoleic acid, and the concentration of described methanol is for 85%.
Specific embodiment 2: present embodiment discloses one and extract linoleic method from Radix seu Cortex Malloti nepalensis crude oil, its feature exists
In, comprise the following steps:
(1) moisten filtration membrane surface with acetone solvent, in crude oil add quality be quality of crude oil be the deionized water of 20%,
At 30 DEG C, pressure 400kPa, by crude oil with flow velocity 0.8m3/h by filtration membrane, described filtration membrane is by polyacrylic acid
Ester resin is made.
(2) in the environment of noble gas, add potassium hydroxide to degummed oil, carry out saponification carrying out be acidified, water
Washing, be dehydrated and obtain fatty acid mixed, wherein the weight fraction of potassium hydroxide is 10%；
(3) by fatty acid mixed freezing 10 hours, rapid sucking filtration after taking-up under the temperature range of 4 DEG C；
(4) adding organic solvent methanol, extract linoleic acid by freeze and separate method, freeze and separate method concretely comprises the following steps: 0
DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 0.5-1.5 hour respectively, by filter type, crystal is separated, enter with oil suction fibre
Row absorption, the product after absorption, be centrifuged at 5 DEG C separate, obtain high-purity linoleic acid, the concentration of described methanol 95%,
The concentration of described acetone is 95%.
Specific embodiment 3: present embodiment discloses one and extract linoleic method from Radix seu Cortex Malloti nepalensis crude oil, its feature exists
In, comprise the following steps:
(1) moisten filtration membrane surface with acetone solvent, in crude oil add quality be quality of crude oil be the deionized water of 15%,
At 20 DEG C, pressure 250kPa, by crude oil with flow velocity 0.5m3/h by filtration membrane, described filtration membrane is by polyurethane tree
Fat is made.
(2) in the environment of noble gas, add sodium hydroxide to degummed oil, carry out saponification carrying out be acidified, water
Washing, be dehydrated and obtain fatty acid mixed, wherein the weight fraction of sodium hydroxide or potassium hydroxide is 15%；
(3) by fatty acid mixed freezing 8 hours, rapid sucking filtration after taking-up under the temperature range of 3 DEG C；
(4) adding organic solvent-acetone and extract linoleic acid by freeze and separate method, freeze and separate method concretely comprises the following steps: 0
DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 1 hour respectively, by filter type, crystal is separated, adsorb with oil suction fibre,
Product after absorption, is centrifuged separating at 0 DEG C, obtains high-purity linoleic acid, and the concentration of described acetone is 85%.
Specific embodiment 4: present embodiment discloses one and extract linoleic method from Radix seu Cortex Malloti nepalensis crude oil, its feature exists
In, comprise the following steps:
(1) moisten filtration membrane surface with acetone solvent, in crude oil add quality be quality of crude oil be the deionization of 10%%
Water, at 30 DEG C, pressure 100kPa, by crude oil with flow velocity 0.6m3/h by filtration membrane, described filtration membrane is by acetic acid
Fiber is made.
(2) in the environment of noble gas, add potassium hydroxide to degummed oil, carry out saponification carrying out be acidified, water
Washing, be dehydrated and obtain fatty acid mixed, wherein the weight fraction of potassium hydroxide is 25%；
(3) by fatty acid mixed freezing 2 hours, rapid sucking filtration after taking-up under the temperature range of 2 DEG C；
(4) adding organic solvent-normal hexane, extract linoleic acid by freeze and separate method, freeze and separate method concretely comprises the following steps: 0
DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 0.5 hour respectively, by filter type, crystal is separated, inhale with oil suction fibre
Attached, after absorption product, is centrifuged separating at 5 DEG C, obtains high-purity linoleic acid, and the concentration of described normal hexane is 95%.
The present embodiment 5: present embodiment discloses one and extract linoleic method from Radix seu Cortex Malloti nepalensis crude oil, its feature exists
In, comprise the following steps:
(1) moisten filtration membrane surface with acetone solvent, in crude oil add quality be quality of crude oil be the deionized water of 15%,
At 12 DEG C, pressure 150kPa, by crude oil with flow velocity 0.8m3/h by filtration membrane, described filtration membrane is by acetate fiber
Make.
(2) in the environment of noble gas, add sodium hydroxide to degummed oil, carry out saponification carrying out be acidified, water
Washing, be dehydrated and obtain fatty acid mixed, wherein the weight fraction of sodium hydroxide is 15%；
(3) by fatty acid mixed freezing 2 hours, rapid sucking filtration after taking-up under the temperature range of about 1 DEG C；
(4) adding organic solvent methanol, extract linoleic acid by freeze and separate method, freeze and separate method concretely comprises the following steps: 0
DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 0.5 hour respectively, by filter type, crystal is separated, inhale with oil suction fibre
Attached, after absorption product, is centrifuged separating at-5 DEG C, obtains high-purity linoleic acid, and the concentration of described methanol is for 95%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (8)
1. one kind is extracted linoleic method from Radix seu Cortex Malloti nepalensis crude oil, it is characterised in that comprise the following steps:
(1) Radix seu Cortex Malloti nepalensis crude oil filters degumming by filtration membrane, obtains degummed oil
(2) in the environment of noble gas, add sodium hydroxide or potassium hydroxide to degummed oil, carry out saponification and go forward side by side
Row is acidified, washes, is dehydrated and obtains fatty acid mixed, and wherein the weight fraction of sodium hydroxide or potassium hydroxide is 10%-30%；
(3) fatty acid mixed is carried out freezing pretreatment；
(4) add organic solvent, extract linoleic acid by freeze and separate method.
The most according to claim 1 from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, it is characterised in that described step 1
Concretely comprising the following steps of membrane filtration degumming: moisten film surface with acetone solvent, in crude oil add quality be quality of crude oil be 10%-
The deionized water of 20%, at 10～30 DEG C, pressure 100～400kPa is thin by filtering with flow velocity 0.2～0.8m3/h by crude oil
Film.
The most according to claim 2 from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, it is characterised in that described step 3
Pretreatment concrete operations are: by fatty acid mixed freezing 2-10 hour under the temperature range of 2 DEG C-4 DEG C, take out rapidly after taking-up
Filter.
The most according to claim 1 from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, it is characterised in that described step 4
The one that organic solvent is methanol, petroleum ether, acetone, normal hexane.
The most according to claim 3 from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, it is characterised in that described methanol
Concentration is at 85-95%.
The most according to claim 3 from Radix seu Cortex Malloti nepalensis crude oil, extract linoleic method, it is characterised in that described acetone
Concentration is at least 85%.
7. according to extracting linoleic method from Radix seu Cortex Malloti nepalensis crude oil one of claim 1-6 Suo Shu, it is characterised in that described
The freeze and separate method of step 4 concretely comprises the following steps: 0 DEG C ,-5 ,-10 ,-20 ,-30 ,-40 freezing 0.5-1.5 hour respectively, pass through
Crystal is separated by filter type, and oil suction fibre adsorbs, the product after absorption, is centrifuged separating, obtains at-5-5 DEG C
High-purity linoleic acid.
8. according to extracting linoleic method from Radix seu Cortex Malloti nepalensis crude oil described in any one of claim 1-6, it is characterised in that institute
The filtration membrane stated is by acetate fiber, polyurethane resin, the one of polyacrylate resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610284304.4A CN105837430A (en) | 2016-05-04 | 2016-05-04 | Method for extracting linoleic acid from idesia polycarpa crude oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610284304.4A CN105837430A (en) | 2016-05-04 | 2016-05-04 | Method for extracting linoleic acid from idesia polycarpa crude oil |
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| CN105837430A true CN105837430A (en) | 2016-08-10 |
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| CN201610284304.4A Pending CN105837430A (en) | 2016-05-04 | 2016-05-04 | Method for extracting linoleic acid from idesia polycarpa crude oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108998207A (en) * | 2018-08-07 | 2018-12-14 | 河南正花食品集团有限公司 | A kind of oil expression method preventing peanut oxidative rancidity |
| CN109022144A (en) * | 2018-06-28 | 2018-12-18 | 广西浙缘农业科技有限公司 | A kind of processing method of oil tea cosmetic base oil |
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| CN101074406A (en) * | 2007-05-30 | 2007-11-21 | 吴江市方霞企业信息咨询有限公司 | Removal of peptized impurities |
| CN101880601A (en) * | 2010-06-25 | 2010-11-10 | 四川省国政生物质能源科技发展股份有限公司 | Method for preparing linoleic acid from idesia polycarpa Maxium. Var. vestita Diels oil |
| CN102320953A (en) * | 2011-07-25 | 2012-01-18 | 四川省毛叶山桐子科技股份有限公司 | Method for preparing natural alpha-linolenic acid from crude oil of idesia polycarpa var.vestita diels |
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2016
- 2016-05-04 CN CN201610284304.4A patent/CN105837430A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074406A (en) * | 2007-05-30 | 2007-11-21 | 吴江市方霞企业信息咨询有限公司 | Removal of peptized impurities |
| CN101880601A (en) * | 2010-06-25 | 2010-11-10 | 四川省国政生物质能源科技发展股份有限公司 | Method for preparing linoleic acid from idesia polycarpa Maxium. Var. vestita Diels oil |
| CN102320953A (en) * | 2011-07-25 | 2012-01-18 | 四川省毛叶山桐子科技股份有限公司 | Method for preparing natural alpha-linolenic acid from crude oil of idesia polycarpa var.vestita diels |
Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109022144A (en) * | 2018-06-28 | 2018-12-18 | 广西浙缘农业科技有限公司 | A kind of processing method of oil tea cosmetic base oil |
| CN108998207A (en) * | 2018-08-07 | 2018-12-14 | 河南正花食品集团有限公司 | A kind of oil expression method preventing peanut oxidative rancidity |
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