CN107353199A - The method of Malania Oleifera Oil separating-purifying nervonic acid - Google Patents

The method of Malania Oleifera Oil separating-purifying nervonic acid Download PDF

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CN107353199A
CN107353199A CN201710680766.2A CN201710680766A CN107353199A CN 107353199 A CN107353199 A CN 107353199A CN 201710680766 A CN201710680766 A CN 201710680766A CN 107353199 A CN107353199 A CN 107353199A
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acid
ether
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saponification
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王显权
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/02Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation

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Abstract

This application discloses a kind of method of Malania Oleifera Oil separating-purifying nervonic acid in chemosynthesis technical field, including 8 steps, Step 1: saponification:The alkali lye that concentration is 10% is added into retort, reaction generates neural acid sodium-salt saponification liquor;Step 2: oil removing;Step 3: acid out:Saponification saline solution is added to acid out tank, it is 6 ~ 7 to stir lower dropwise addition sulfuric acid to pH, separates out white and mixes acid out liquid;Step 4: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, saltcake solution is filtered off and remove wastewater disposal basin, collected standby after mixing acid heat water washing air-dries;Step 5: ether dissolved;Step 6: acetone dissolved;Step 7: petroleum ether dissolved;Step 8: processing obtains nervonic acid.The present invention, as three subcrystalline solvents, obtains the nervonic acid of high purity 85%, the rate of recovery more than 52% using ether, acetone and petroleum ether;It is with short production cycle and technique is simple to operation, it is environment-friendly, it is adapted to industrialized production.

Description

The method of Malania Oleifera Oil separating-purifying nervonic acid
Technical field
The present invention relates to chemosynthesis technical field, and in particular to a kind of method of Malania Oleifera Oil separating-purifying nervonic acid.
Background technology
Malania oleifera, after scientific name MalaniaoleiferaetLee, also known as mountain paulownia fruit, Tieghemella heckelii Pierre, wild paulownia, kalimeris etc..Rascal Section, woody Chang Green tallow trees.Tree trunk is straight, up to 20 meters, and tree-walk oval leaf, oblate spheroid tree fruit, is grown in 500- up to 40 centimetres In 1640 meters of fertile Limestone Mountain mixed forests of moistening.South China production tung oil area town and country can be used as greening-tree, landscape tree, oil Material tree plant.Autumn and winter harvest fruit, and frying eats into Malania Oleifera Oil and makees iundustrial oil, tree trunk matter is close preferably to make timber.
Soap thing content is not 4% to Malania Oleifera Oil in Malania Oleifera Oil grease;Nervonic acid, content 67%;Containing oleic acid(12%)It is and micro- The acid such as capric acid, laurate, myristic acid, palmitic acid are measured, undeterminate composition is 14%.
Wherein tetracosenoic acid, also known as nervonic acid, molecular structural formula:H3(CH2)7CH=CH(CH2)13COOH, Yi Zhongbai Color crystallizes, and relative molecular mass 366.6, can be dissolved in alcohol, not soluble in water, 39~40 DEG C of fusing point.Nervonic acid is scientists from all over the world Generally acknowledged can repair dredging injured brain nerve pathway --- nerve fibre, and the economic benefits and social benefits material for promoting nerve cell to regenerate.God The core natural component of cerebral nerve fiber and nerve cell through acid, the shortage of nervonic acid will cause cerebral apoplexy sequela, The cerebral diseases such as senile dementia, brain paralysis, encephalatrophy, failure of memory, insomnia forgetfulness, and nervonic acid human body itself is difficult synthesis, must It must be supplemented by food intake, therefore nervonic acid is a kind of chemical products for the needed by human body that reaction must be relied on to prepare.
It is reported that the relevant report of extraction separation nervonic acid is less from Malania Oleifera Oil.Hao Xuya etc. is " in Malania Oleifera Oil The nervonic acid in Malania Oleifera Oil is separated using urea adduct method in the separating-purifying research of nervonic acid " paper, urea Inclusion method is dissolved urea in organic solvent, and when adding aliphatic acid, hexahedral structure is formed with hydrogen bond between urea molecule, Spiral helicine inclusion compound framework is formed, because the diameter of saturated fatty acid is less than the free space of framework, in crystallization process, directly The saturated fatty acid of chain or monounsaturated fat enter in framework, by urea clathrate, form inclusion compound and separate out.And how unsaturated Aliphatic acid is not easy by urea clathrate, based on above-mentioned principle, you can by unrighted acid(Ester)With saturated fatty acid(Ester)Separate, When i.e. in Malania Oleifera Oil, inclusion removes the aliphatic acid of the low-carbons such as oleic acid, so as to isolate nervonic acid.But time of this method Yield is low(Only 46.8%), purity is also low(Only 65%).
The content of the invention
The invention is intended to provide a kind of technique of the extraction separation nervonic acid from Malania Oleifera Oil, to solve prior art separation The problem of method of purification rate of recovery is low, and purity is low.
The technical scheme is that the method for Malania Oleifera Oil separating-purifying nervonic acid, comprises the following steps:
Step 1: saponification:The alkali lye that concentration is 10% is added into retort, Malania Oleifera Oil is added in retort afterwards, stirred Mix, be passed through and be steam heated to 70 ~ 80 DEG C, persistently add alkali lye, disappeared to fluid, reaction generates neural acid sodium-salt saponification liquor;
Step 2: oil removing:Saponification liquor cools down, and adds ether and neural acid sodium-salt saponification liquor is extracted, stand, separate upper strata ether Liquid, ether is reclaimed, Residual oil is discarded, stays saponification saline solution;
Step 3: acid out:Saponification saline solution is added to acid out tank, stir and be added dropwise sulfuric acid that concentration is 10% to pH be 6 ~ 7, analysis Go out white and mix acid out liquid;
Step 4: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, the sodium sulphate of filtering reaction generation removes waste water Pond, filtrate are mixed acid, standby after then air-drying with hot wash mixed acid;
Step 5: ether dissolved:Acid will be mixed to be added in the ether of 3 times of weight, be dissolved as ether acid solution, suction strainer goes out immiscible acid (1), ether acid solution is cooled at -10 ~ -5 DEG C and crystallized, and suction strainer goes out brilliant sour (2), and ether mother liquor steams recovery ether, stays steaming spent acid (3);
Step 6: acetone dissolved:Brilliant acid (2) is added in 3 times of weight acetones, is dissolved as acetone acid solution, suction strainer goes out immiscible acid (4), acetone acid solution, which is cooled at -10 ~ -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid(5), acetone mother liquor steams recovery acetone, stays steaming spent acid (6);
Step 7: petroleum ether dissolved:Brilliant acid (5) is added in 3 times of weight petroleum ethers, is dissolved as petroleum ether acid solution, suction strainer goes out not Molten acid (7), petroleum ether acid solution, which is cooled at -10 ~ -5 DEG C, to be crystallized, and suction strainer goes out brilliant sour (8), and petroleum ether mother liquor steams recovery petroleum ether, Stay and steam spent acid (9);
Step 8: processing:Brilliant acid (8) be nervonic acid, merge immiscible acid (1), immiscible acid (4), immiscible acid (7), steaming spent acid (3), Steam spent acid (6) and steam spent acid (9), separately comprehensively utilize.
The working principle and beneficial effect of the present invention:The present invention uses the malania oleifera rich in nervonic acid as raw material, and is directed to Tradition extraction from malania oleifera separates existing above mentioned problem during nervonic acid, and saponification is generated using first saponification Liquid, then saponification liquor is removed into the not miscellaneous oil of soap, by adding sulfuric acid acid out into fatty acid mixed, air-dried by hot wash after filtering Pure mixing-in fat acid crystal is obtained afterwards, is started dissolved afterwards and is crystallized three times;Crystallization for the first time uses ether as solvent, first Immiscible acid is removed through suction strainer(4), then ether acid solution is cooled at -10 ~ -5 DEG C and crystallized, continue suction strainer and obtain brilliant acid(2), suction strainer After ether mother liquor afterwards steams ether, residue steams spent acid(3);Second of crystallization first removes not by the use of acetone as solvent through suction strainer Molten acid(5), then acetone acid solution is cooled at -10 ~ -5 DEG C and crystallized, continued suction strainer and obtain brilliant acid 5, the acetone mother liquor after suction strainer steams After going out acetone, residue steams spent acid(6);Third time crystallization first removes immiscible acid by the use of petroleum ether as solvent through suction strainer(7), then will Petroleum ether acid solution is cooled at -10 ~ -5 DEG C and crystallized, and continues suction strainer and obtains brilliant acid(8), the petroleum ether mother liquor after suction strainer steams oil After ether, residue steams spent acid(9);Repeated recrystallize is carried out to aliphatic acid more than, final arrives pure white needle-like crystals Nervonic acid, through gas chromatographic analysis, the purity of nervonic acid is more than 85%, and the rate of recovery is up to 52%.The present invention using ether, acetone and For petroleum ether as three subcrystalline solvents, gradual sub-department includes oleic acid, capric acid, laurate, myristic acid, palmitic acid and not Other acid of measure, are further purified to it, obtain the nervonic acid of high purity 85%, the rate of recovery is more than 52%.This The method of invention is quick, efficient, noresidue, and technique is simple to operation, with short production cycle, environment-friendly, is adapted to industrial metaplasia Production.
Further, during the step 5 ether dissolved, ether acid solution, which is cooled at -5 DEG C, to be crystallized.Crystallize at such a temperature, god Purity through acid can improve 3%.
Further, during the step 6 acetone dissolved, acetone acid solution, which is cooled at -5 DEG C, to be crystallized.Crystallize at such a temperature, god Purity through acid can improve 3%.
Further, during the step 7 petroleum ether dissolved, 10% absolute ethyl alcohol is added in petroleum ether, mixed Petroleum ether acid solution, brilliant acid 5 is added in the mixing petroleum ether acid solution of 3 times of weight afterwards, is cooled at -5 DEG C and crystallizes.Add anhydrous Crystallized at such a temperature after ethanol, the purity of nervonic acid can improve 5%.
As the further preferred of this programme, before step 1 saponification starts, Malania Oleifera Oil is first subjected to molecular distillation, Vapo(u)rizing temperature is 150 DEG C, distillation pressure 11Pa, obtains light component and heavy constituent, light component and heavy constituent carry out saponification respectively And subsequent treatment.Molecular distillation is first passed through, weight component is separated, carries out saponification and the processing of follow-up recrystallization respectively, The nervonic acid of different purity is respectively obtained, the nervonic acid purity highest wherein obtained after light component saponification and subsequent treatment, is up to 95%, it is mainly used in the industries such as health care and food;And the nervonic acid purity that heavy constituent obtains is taken second place, 90% or so.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the embodiment of the method 3 of Malania Oleifera Oil separating-purifying nervonic acid of the present invention.
Embodiment
Below by embodiment, the present invention is further detailed explanation:
Embodiment 1:The method of Malania Oleifera Oil separating-purifying nervonic acid, is concretely comprised the following steps:
Step 1: saponification:The sodium hydroxide that concentration is 10% is added into retort, afterwards adds Malania Oleifera Oil in retort, Stirring, is passed through and is steam heated to 70 ~ 80 DEG C, persistently adds the sodium hydroxide that concentration is 10%, is disappeared to a large amount of fluid, reaction life Generating nervous acid sodium salt saponification liquor, now pH=8 of solution;
Step 2: oil removing:Saponification liquor cools down, and soap oil is not miscellaneous in addition ether extraction saponification liquid, stands, separates upper strata ether solution, Ether is reclaimed, Residual oil is discarded, stays saponification saline solution;
Step 3: acid out:Saponification saline solution is added to acid out tank, the sulfuric acid that dropwise addition concentration is 10% under stirring to pH is 6 ~ 7, analysis Go out white and mix acid out liquid;
Step 4: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, metabisulfite solution is filtered off and remove wastewater disposal basin, collect Mix standby after acid heat water washing air-dries;
Step 5: ether dissolved:Mixing sour be added in the ether of 3 times of weight and be dissolved as ether acid solution, suction strainer goes out immiscible acid 1, Ether acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 2, and ether mother liquor steams recovery ether, stays ether mother liquor spent acid 3;
Step 6: acetone dissolved:Brilliant acid 2, which is added in 3 times of weight acetones, is dissolved as acetone acid solution, and suction strainer goes out immiscible acid 4, acetone Acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 5, and acetone mother liquor steams recovery acetone;Stay acetone mother liquor spent acid 6;
Step 7: petroleum ether dissolved:It is solution that brilliant acid 5, which is added to 3 times of weight petroleum ether dissolutions, and suction strainer goes out immiscible acid 7, petroleum ether Acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 8, and petroleum ether mother liquor steams recovery petroleum ether;Stay and steam spent acid 9;
Step 8: processing:Processing:Brilliant acid 8 be nervonic acid, merging immiscible acid 1, immiscible acid 4, immiscible acid 7, ether mother liquor spent acid 3, Acetone mother liquor spent acid 6 and petroleum ether mother liquor spent acid 9, are separately comprehensively utilized.
Embodiment 2:The method of Malania Oleifera Oil separating-purifying nervonic acid, is concretely comprised the following steps:
Step 1: saponification:The sodium hydroxide that concentration is 10% is added into retort, afterwards adds Malania Oleifera Oil in retort, Stirring, is passed through and is steam heated to 70 ~ 80 DEG C, persistently adds the sodium hydroxide that concentration is 10%, is disappeared to a large amount of fluid, reaction life Generating nervous acid sodium salt saponification liquor, now pH=8 of solution;
Step 2: oil removing:Saponification liquor cools down, and soap oil is not miscellaneous in addition ether extraction saponification liquid, stands, separates upper strata ether solution, Ether is reclaimed, Residual oil is discarded, stays saponification saline solution;
Step 3: acid out:Saponification saline solution is added to acid out tank, the sulfuric acid that dropwise addition concentration is 10% under stirring to pH is 6 ~ 7, analysis Go out white and mix acid out liquid;
Step 4: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, metabisulfite solution is filtered off and remove wastewater disposal basin, collect Mix standby after acid heat water washing air-dries;
Step 5: ether dissolved:Mixing sour be added in the ether of 3 times of weight and be dissolved as ether acid solution, suction strainer goes out immiscible acid 1, Ether acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 2, and ether mother liquor steams recovery ether, stays ether mother liquor spent acid 3;
Step 6: acetone dissolved:Brilliant acid 2, which is added in 3 times of weight acetones, is dissolved as acetone acid solution, and suction strainer goes out immiscible acid 4, acetone Acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 5, and acetone mother liquor steams recovery acetone;Stay acetone mother liquor spent acid 6;
Step 7: petroleum ether dissolved:Petroleum ether liquid is configured, by 10% absolute ethyl alcohol into petroleum ether, obtains mixing oil ether acid Liquid, brilliant acid 5 being added to 3 times of weight and mixed in petroleum ether acid solutions afterwards and is dissolved, suction strainer goes out immiscible acid 7, and petroleum ether acid solution is cooled to- Crystallized at 5 DEG C, suction strainer goes out brilliant acid 8, and petroleum ether mother liquor steams recovery petroleum ether;Stay petroleum ether mother liquor spent acid 9;
Step 8: processing:Processing:Brilliant acid 8 be nervonic acid, merging immiscible acid 1, immiscible acid 4, immiscible acid 7, ether mother liquor spent acid 3, Acetone mother liquor spent acid 6 and petroleum ether mother liquor spent acid 9, are separately comprehensively utilized.
Embodiment 3:Referring to Fig. 1, the method for Malania Oleifera Oil separating-purifying nervonic acid, concretely comprise the following steps:
Step 1: molecular distillation:Malania Oleifera Oil is first subjected to molecular distillation, vapo(u)rizing temperature is 150 DEG C, distillation pressure 11Pa, Light component and heavy constituent are obtained, light component and heavy constituent carry out the operation of two ~ step 9 of following step respectively.
Step 2: saponification:The sodium hydroxide that concentration is 10% is added into retort, afterwards by a kind of light component of step Or the Malania Oleifera Oil of heavy constituent is added in retort, stirring, it is passed through and is steam heated to 70 ~ 80 DEG C, persistently adds concentration as 10% Sodium hydroxide, disappeared to a large amount of fluid, reaction generates neural acid sodium-salt saponification liquor, now pH=8 of solution;
Step 3: oil removing:Saponification liquor cools down, and soap oil is not miscellaneous in addition ether extraction saponification liquid, stands, separates upper strata ether solution, Ether is reclaimed, Residual oil is discarded, stays saponification saline solution;
Step 4: acid out:Saponification saline solution is added to acid out tank, the sulfuric acid that dropwise addition concentration is 10% under stirring to pH is 6 ~ 7, analysis Go out white and mix acid out liquid;
Step 5: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, metabisulfite solution is filtered off and remove wastewater disposal basin, collect Mix standby after acid heat water washing air-dries;
Step 6: ether dissolved:Mixing sour be added in the ether of 3 times of weight and be dissolved as ether acid solution, suction strainer goes out immiscible acid 1, Ether acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 2, and ether mother liquor steams recovery ether, stays ether mother liquor spent acid 3;
Step 7: acetone dissolved:Brilliant acid 2, which is added in 3 times of weight acetones, is dissolved as acetone acid solution, and suction strainer goes out immiscible acid 4, acetone Acid solution, which is cooled at -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid 5, and acetone mother liquor steams recovery acetone;Stay acetone mother liquor spent acid 6;
Step 8: petroleum ether dissolved:Petroleum ether liquid is configured, 10% absolute ethyl alcohol is added in petroleum ether, obtains mixing oil Ether acid liquid, brilliant acid 5 is added to 3 times of weight and mixed in petroleum ether acid solution afterwards and is dissolved, suction strainer goes out immiscible acid 7, petroleum ether acid solution It is cooled at -5 DEG C and crystallizes, suction strainer goes out brilliant acid 8, and petroleum ether mother liquor steams recovery petroleum ether;Stay petroleum ether spent acid 9;
Step 9: processing:Brilliant acid 8 is nervonic acid, merges immiscible acid 1, immiscible acid 4, immiscible acid 7, ether mother liquor spent acid 3, acetone Mother liquor spent acid 6 and petroleum ether mother liquor spent acid 9, are separately comprehensively utilized.
100g Malania Oleifera Oil is chosen as experimental raw, respectively using urea adduct method and embodiments of the invention 1 ~ 3 Experiment contrast analysis is carried out, conclusion is as follows:
Table 1 is analyzed to crystallize lower purity and the rate of recovery three times
The rate of recovery of different number crystallizations is equal to weight component sum wherein in embodiment 3.
Referring to above-mentioned purity and rate of recovery value, 1 ~ embodiment of embodiments of the invention 3 is above urea of the prior art Inclusion method, wherein especially with by molecular distillation and third time crystallize after add absolute ethyl alcohol obtain nervonic acid purity highest.
Above-described is only embodiments of the invention, and the general knowledge such as known concrete structure and characteristic is not made herein in scheme Excessive description., without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art Several modifications and improvements are made, these should also be considered as protection scope of the present invention, and these are implemented all without the influence present invention Effect and practical applicability.The scope of protection required by this application should be based on the content of the claims, in specification The records such as embodiment can be used for the content for explaining claim.

Claims (5)

1. the method for Malania Oleifera Oil separating-purifying nervonic acid, it is characterised in that comprise the following steps:
Step 1: saponification:The alkali lye that concentration is 10% is added into retort, Malania Oleifera Oil is added in retort afterwards, stirred Mix, be passed through and be steam heated to 70 ~ 80 DEG C, persistently add alkali lye, disappeared to fluid, reaction generates neural acid sodium-salt saponification liquor;
Step liquid extracts, and stands, and separates upper strata ether solution, reclaims ether, discards Residual oil, stay saponification saline solution;
Step 3: acid out:Saponification saline solution is added to acid out tank, stir and be added dropwise sulfuric acid that concentration is 10% to pH be 6 ~ 7, analysis Go out white and mix acid out liquid;
Step 4: acid filtering:Acid out liquid will be mixed to be put into the filter pocket for being covered with filter cloth, the sodium sulphate of filtering reaction generation removes waste water Pond, filtrate are mixed acid, standby after then air-drying with hot wash mixed acid;
Step 5: ether dissolved:Acid will be mixed to be added in the ether of 3 times of weight, be dissolved as ether acid solution, suction strainer goes out immiscible acid (1), ether acid solution is cooled at -10 ~ -5 DEG C and crystallized, and suction strainer goes out brilliant sour (2), and ether mother liquor steams recovery ether, stays steaming spent acid (3);
Step 6: acetone dissolved:Brilliant acid (2) is added in 3 times of weight acetones, is dissolved as acetone acid solution, suction strainer goes out immiscible acid (4), acetone acid solution, which is cooled at -10 ~ -5 DEG C, to be crystallized, and suction strainer goes out brilliant acid(5), acetone mother liquor steams recovery acetone, stays steaming spent acid (6);
Step 7: petroleum ether dissolved:Brilliant acid (5) is added in 3 times of weight petroleum ethers, is dissolved as petroleum ether acid solution, suction strainer goes out not Molten acid (7), petroleum ether acid solution, which is cooled at -10 ~ -5 DEG C, to be crystallized, and suction strainer goes out brilliant sour (8), and petroleum ether mother liquor steams recovery petroleum ether, Stay and steam spent acid (9);
Step 8: processing:Brilliant acid (8) be nervonic acid, merge immiscible acid (1), immiscible acid (4), immiscible acid (7), steaming spent acid (3), Steam spent acid (6) and steam spent acid (9), separately comprehensively utilize.
2. the method for Malania Oleifera Oil separating-purifying nervonic acid according to claim 1, it is characterised in that:The step 5 second During ether dissolved, ether acid solution, which is cooled at -5 DEG C, to be crystallized.
3. the method for Malania Oleifera Oil separating-purifying nervonic acid according to claim 2, it is characterised in that:The step 6 third During ketone dissolved, acetone acid solution, which is cooled at -5 DEG C, to be crystallized.
4. the method for Malania Oleifera Oil separating-purifying nervonic acid according to claim 3, it is characterised in that:The step 7 stone During oily ether dissolved, 10% absolute ethyl alcohol is added in petroleum ether, obtains mixing petroleum ether acid solution, is afterwards added to brilliant acid 5 In the mixing petroleum ether acid solution of 3 times of weight, it is cooled at -5 DEG C and crystallizes.
5. the method for described Malania Oleifera Oil separating-purifying nervonic acid according to claim 4, it is characterised in that:In step 1 Before starting saponification, Malania Oleifera Oil is first subjected to molecular distillation, vapo(u)rizing temperature is 150 DEG C, distillation pressure 11Pa, obtains light group Divide and heavy constituent, light component and heavy constituent carry out saponification and subsequent treatment respectively.
CN201710680766.2A 2017-08-10 2017-08-10 The method of Malania Oleifera Oil separating-purifying nervonic acid Pending CN107353199A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863764A (en) * 2018-07-20 2018-11-23 李明龙 A kind of improvement memory improves the nervonic acid piece preparation method of sleep quality
CN111117773A (en) * 2019-12-25 2020-05-08 昆明酷特利生物科技有限公司 Method for separating nervonic acid from garlic oil and application thereof
CN112174811A (en) * 2020-08-27 2021-01-05 菏泽中禾健元生物科技有限公司 High-efficiency high-purity extraction process of nervonic acid, namely cis-15-tetracosenic acid

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1398844A (en) * 2002-09-04 2003-02-26 杭州施惠泰食品化学有限公司 Nervonic acid extracting and purifying production process
CN1609090A (en) * 2003-10-23 2005-04-27 杨凌元宝枫生物制品有限公司 Technological process of extracting nervonic acid from Acertruncatum Bunge oil
CN1775732A (en) * 2005-11-22 2006-05-24 陕西宝枫科技股份有限公司 Method for extracting nervonic acid from acer truncatum buge oil
CN105037133A (en) * 2015-08-17 2015-11-11 浙江大学 Method of extracting nervonic acid from malania oleifera
CN105503580A (en) * 2015-12-09 2016-04-20 江西青春康源制药有限公司 Method for extracting and separating nervonic acid
CN106397384A (en) * 2016-08-30 2017-02-15 昆明酷特利生物科技有限公司 Method for synthesis of macrocyclic musk lactone
CN106397160A (en) * 2016-08-30 2017-02-15 昆明酷特利生物科技有限公司 Synthetic method for macrocyclic musk ketone
CN106496026A (en) * 2016-10-21 2017-03-15 武汉藤欣生物工程有限公司 In the method that acer truncatum buge oil prepares neural acetoacetic ester as raw material
CN106565662A (en) * 2016-10-26 2017-04-19 西南林业大学 Method for preparing macrocyclic musk-cyclopentadecanolide from malania oleifera oil

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1398844A (en) * 2002-09-04 2003-02-26 杭州施惠泰食品化学有限公司 Nervonic acid extracting and purifying production process
CN1609090A (en) * 2003-10-23 2005-04-27 杨凌元宝枫生物制品有限公司 Technological process of extracting nervonic acid from Acertruncatum Bunge oil
CN1775732A (en) * 2005-11-22 2006-05-24 陕西宝枫科技股份有限公司 Method for extracting nervonic acid from acer truncatum buge oil
CN100341839C (en) * 2005-11-22 2007-10-10 陕西宝枫科技股份有限公司 Method for extracting nervonic acid from acer truncatum buge oil
CN105037133A (en) * 2015-08-17 2015-11-11 浙江大学 Method of extracting nervonic acid from malania oleifera
CN105037133B (en) * 2015-08-17 2017-06-30 浙江大学 A kind of method that nervonic acid is extracted from malania oleifera
CN105503580A (en) * 2015-12-09 2016-04-20 江西青春康源制药有限公司 Method for extracting and separating nervonic acid
CN105503580B (en) * 2015-12-09 2017-07-21 江西青春康源制药有限公司 A kind of extraction separation method of nervonic acid
CN106397384A (en) * 2016-08-30 2017-02-15 昆明酷特利生物科技有限公司 Method for synthesis of macrocyclic musk lactone
CN106397160A (en) * 2016-08-30 2017-02-15 昆明酷特利生物科技有限公司 Synthetic method for macrocyclic musk ketone
CN106496026A (en) * 2016-10-21 2017-03-15 武汉藤欣生物工程有限公司 In the method that acer truncatum buge oil prepares neural acetoacetic ester as raw material
CN106565662A (en) * 2016-10-26 2017-04-19 西南林业大学 Method for preparing macrocyclic musk-cyclopentadecanolide from malania oleifera oil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周琴芬: "蒜头果种仁神经酸制备工艺研究", 《浙江大学硕士学位论文》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863764A (en) * 2018-07-20 2018-11-23 李明龙 A kind of improvement memory improves the nervonic acid piece preparation method of sleep quality
CN111117773A (en) * 2019-12-25 2020-05-08 昆明酷特利生物科技有限公司 Method for separating nervonic acid from garlic oil and application thereof
CN111117773B (en) * 2019-12-25 2022-12-09 昆明酷特利生物科技有限公司 Method for separating nervonic acid from garlic oil and application thereof
CN112174811A (en) * 2020-08-27 2021-01-05 菏泽中禾健元生物科技有限公司 High-efficiency high-purity extraction process of nervonic acid, namely cis-15-tetracosenic acid

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