CN1837182A - Process for preparing alpha-ethyl linolenate with purity more than 80% - Google Patents
Process for preparing alpha-ethyl linolenate with purity more than 80% Download PDFInfo
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- CN1837182A CN1837182A CN 200510107355 CN200510107355A CN1837182A CN 1837182 A CN1837182 A CN 1837182A CN 200510107355 CN200510107355 CN 200510107355 CN 200510107355 A CN200510107355 A CN 200510107355A CN 1837182 A CN1837182 A CN 1837182A
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Abstract
The invention relates to a process for preparing alpha-zinc linolenate by using perilla seeds as the raw material, which comprises the steps of squeezing, filtering, saponifying, acidifying, water scrubbing, urea complexing, freezing, filter-pressing, elevating temperature, extracting, esterifying, water scrubbing, dewatering, and vacuum distilling. The obtained product has a purity of over 80%.
Description
Technical field
The present invention relates to a kind of is that raw material production goes out the production technique of purity greater than 80% Alpha-ethyl linolenate with the perilla seed.
Background technology
Alpha-linolenic acid mainly is present in the various plants grease with the triglyceride level form, comprise linseed oil, Purple Perilla Seed Oil, rape seed oil, Oleum Gossypii semen, soybean wet goods, wherein content is up to 50%～60% in linseed oil, the Purple Perilla Seed Oil, and content is all below 10% in other oil.To unsaturated fatty acids famine, particularly alpha-linolenic acid, need to replenish among the crowd from other approach.Many as adding use in medicine, food service industry, because alpha-linolenic acid purity is lower in the nature species, the interpolation that has influenced alpha-linolenic acid is used, the existence form of ethyl ester is stable than free acid, be convenient to scale operation and use, and the domestic technology of still not having production purity greater than 80% Alpha-ethyl linolenate.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art and the production technique of a kind of purity greater than 80% Alpha-ethyl linolenate is provided.
The object of the present invention is achieved like this:
Carry out according to following technology:
The first step: oil expression: adopt mechanical cold pressing process to squeeze perilla oil perilla seed,
Second step: filter: the solid impurity in the perilla oil is leached,
The 3rd step: saponification: the second step gained perilla oil and deionized water, enzyme catalyst (lipolase100L) are added in the container according to the ratio of weight ratio 1: 0.5～4: 0.01～0.1; stir and heating; the control temperature of charge is between 40 ℃～70 ℃; control material pH value is 7; reaction times was at 2～20 hours; reaction finishes, the omnidistance logical nitrogen protection of this process
The 4th step: acidifying: be in the material after 10%～90% sulfuric acid slowly adds the saponification of the 3rd step gained with concentration and stir; control material reaction temperature is between 40 ℃～95 ℃; when the pH value of material stops to add sulfuric acid less than 4 the time; when the pH value of material greater than 4 the time, continue slowly to add sulfuric acid, repeat aforesaid operations; when the pH value of material less than 4 keep 2 hours constant after; reaction finishes, the omnidistance logical nitrogen protection of this process
The 5th step: washing: the 4th step gained material was left standstill 1～6 hour; emit lower aqueous solution, in remaining upper strata lipid acid, add 0.5～4 times deionized water, stir; left standstill 1～6 hour; emitting lower aqueous solution again, repeat aforesaid operations, is 7 until the lower aqueous solution pH value of emitting; upper strata lipid acid enters next procedure; this end of processing, the omnidistance logical nitrogen protection of this process
The 6th step: urea complexation: with the lipid acid of the 5th step gained, 70%～99.9% edible ethanol, urea by weight 1: (1～8): the ratio of (1～8) adds container and stirs; controlled temperature is between 60 ℃～100 ℃; 0.5～8 hour hold-time; then material is cooled to 20 ℃～60 ℃; this operation finishes; the omnidistance logical nitrogen protection of this operation
The 7th step: freezing: the material of the 6th step gained is carried out the stage cooling; fs is reduced to 0 ℃ from original temperature; subordinate phase is reduced to (5～-10 ℃) from 0 ℃; phase III is reduced to (10～-20 ℃) from (5～-10 ℃); the quadravalence section is reduced to (20～-30 ℃) from (10～-20 ℃); five-stage is reduced to (30～-40 ℃) from (20～-30 ℃); the 6th stage was reduced to (40～-50 ℃) from (30～-40 ℃); per stage need be incubated 0.5～8 hour; the uninterrupted stirring, when temperature reached requirement, this operation finished; the omnidistance logical nitrogen protection of this operation
The 8th step: press filtration: the 7th step gained material is realized solid-liquid separation with pressure and filtering net under 0 ℃～-50 ℃ states, liquid enters next procedure,
The 9th step: heat up: the material of the 8th step gained is warming up to 10 ℃～30 ℃, the omnidistance nitrogen protection of this operation,
The tenth goes on foot: extraction: with the material and deionized water 1: 0.5～4 the mixed and the stirring by weight of the 9th step gained, standing demix is emitted lower aqueous solution, and upper strata lipid acid enters next procedure, the omnidistance nitrogen protection of this operation,
The tenth-step: esterification: with the lipid acid of the tenth step gained, 85%～99.9% edible ethanol, 50%～98% sulfuric acid by weight 1: (0.2～2): the mixed of (0.05～0.1) adds in the container, between 70 ℃～100 ℃ of the control reaction temperature, 4～20 hours time, emit lower floor's solution after the cooling, repeat aforesaid operations, analyze acid number less than 10mgKOH/g until upper strata fatty-acid ethyl ester sample thief, this operation finishes.The upper strata fatty-acid ethyl ester enters next procedure.
The 12 step: washing: the 11 step fatty-acid ethyl ester of gained and the deionized water ratio by weight 1: 0.5～4 entered mix in the container; standing demix; discharge lower layer of water; repeat aforesaid operations; until the lower layer of water pH value is 7; the upper strata fatty-acid ethyl ester enters next procedure, the omnidistance nitrogen protection of this operation
The 13 step: dehydration: the fatty-acid ethyl ester of the 12 step gained was distilled 1～4 hour under the condition of 20 ℃～80 ℃ of vacuum 400～700mmHg, temperature,
The 14 step: molecular distillation: the fatty-acid ethyl ester of the 13 step gained is sent into international advanced complete molecular distillation apparatus (outsourcing), control pressure is between 0.1～5Pa, 80 ℃～150 ℃ of temperature, decolouring flavor is handled, and produces purity greater than 80% Alpha-ethyl linolenate product.
The present invention has following positively effect: the present invention has that purity height, cost are low, the advantage of long quality-guarantee period, utilize this technology can successfully realize the production of purity greater than 80% Alpha-ethyl linolenate product, make the interpolation approach of Alpha-ethyl linolenate more extensive, make the crowd better replenish Alpha-ethyl linolenate simultaneously, promoted that effectively the crowd is healthy, the quality product that the present invention prepares meets the provisions of the relevant regulations issued by the State, and is better than domestic product of the same type.
The every index of product is as follows
The Oranoleptic indicator
| Project | Requirement |
| Color and luster | Colourless-faint yellow |
| Impurity | The visible tramp material of no naked eyes |
| Transparency | Allow little turbid |
Physical and chemical index
| Alpha-linolenic acid second fat % 〉= | 80 |
| Linolic acid % 〉= | 15 |
| Oleic acid %≤ | 5 |
| Stearic acid %≤ | 0.3 |
| Acid value mgKOH/g≤ | 10 |
| Moisture %≤ | 0.1 |
| Peroxide value %≤ | 0.15 |
Microbiological indicator
| Project | Index |
| Total number of bacterial colony, cfu/g≤ | 1000 |
| Coliform, MPN/100g≤ | 40 |
| Mould, cfu/g≤ | 25 |
| Yeast, cfu/g≤ | 25 |
| Salmonellas | Must not detect |
| Shigellae | Must not detect |
| Streptococcus aureus | Must not detect |
| Hemolytic streptococcus | Must not detect |
Embodiment
Embodiment 1: with 300 kilograms of perilla seeds is that raw material is processed.
The first step: oil expression: 300 kilograms of perilla seeds, adopt mechanical cold pressing process to squeeze perilla oil,
Second step: filter: the solid impurity in the perilla oil is leached, get 100 kilograms of perilla oils,
The 3rd step: saponification: get 100 kilograms of perilla oils; 50 kilograms of deionized waters; in 1 kilogram of adding container of enzyme catalyst (lipolase100L), stir and heating 40 ℃ of control temperature of charge; control material pH value is 7; reaction times, sample thief was analyzed acid number at 2 hours, and reaction finishes when acid number reaches 120～210mgKOH/g; the omnidistance logical nitrogen protection of this process
The 4th step: acidifying: be in the material after 10% sulfuric acid slowly adds the saponification of the 3rd step gained with concentration and stir; 40 ℃ of control material reaction temperature; when the pH value of material is stopping to add sulfuric acid less than 4 the time; when the pH value of material greater than 4 the time, continue slowly to add sulfuric acid, repeat aforesaid operations; when the pH value of material less than 4 keep 2 hours constant after; reaction finishes, the omnidistance logical nitrogen protection of this process
The 5th step: washing: the 4th step gained material was left standstill 1 hour, emit lower aqueous solution, get 50 kilograms in lipid acid; the deionized water that in lipid acid, adds 25 kilograms; stir, left standstill 1 hour, emit lower aqueous solution again; repeat aforesaid operations; until the lower aqueous solution pH value of emitting is 7, gets upper strata lipid acid and enters next procedure, this end of processing for 48 kilograms; the omnidistance logical nitrogen protection of this process
The 6th step: urea complexation: with 48 kilograms in the lipid acid of the 5th step output, 48 kilograms of 70% edible ethanols, 48 kilograms of adding containers of urea stir; controlled temperature 0.5 hour hold-time, is cooled to 20 ℃ to material then at 60 ℃; this operation finishes, the omnidistance logical nitrogen protection of this operation
The 7th step: freezing: the material in the 6th step is carried out the stage cooling, and the fs is reduced to 0 ℃ from original temperature, and subordinate phase is reduced to-5 ℃ from 0 ℃; phase III is reduced to-10 ℃ from-5 ℃; the quadravalence section is reduced to-20 ℃ from-10 ℃, and five-stage is reduced to-30 ℃ from-20 ℃, and the 6th stage was reduced to-40 ℃ from-30 ℃); per stage insulation 0.5 hour; the uninterrupted stirring, when temperature reached requirement, this operation finished; the omnidistance logical nitrogen protection of this operation
The 8th step: press filtration: the 7th step gained material is realized solid-liquid separation with pressure and filtering net under 0 ℃ of state, get 42 kilograms of liquid materials, liquid material enters next procedure,
The 9th step: heat up: the material of the 8th step gained is warming up to 10 ℃, the omnidistance nitrogen protection of this operation,
The tenth goes on foot: extraction: the material and the deionized water of the 9th step gained are mixed and stir for 21 kilograms, and standing demix is emitted lower aqueous solution, and get upper strata lipid acid and enter next procedure for 6 kilograms, the omnidistance nitrogen protection of this operation,
The 11 step: esterification: 6 kilograms in the lipid acid of the tenth step gained, 85% 1.2 kilograms of edible ethanols, 50% sulfuric acid mixed for 0.3 kilogram add in the container, 70 ℃ of control reaction temperature, 4 hours time, emit lower floor's solution after the cooling, repeat aforesaid operations, analyze acid number less than 10mgKOH/g until upper strata fatty-acid ethyl ester sample thief, this operation finishes.Get the upper strata fatty-acid ethyl ester and enter next procedure for 6 kilograms,
The 12 step: washing: the fatty-acid ethyl ester of the tenth step gained being added 3 kilograms of mixing of deionized water, leave standstill, discharge lower layer of water, repeat aforesaid operations, is 7 until the lower layer of water pH value, and the upper strata fatty-acid ethyl ester enters next procedure, the omnidistance nitrogen protection of this operation,
The 13 step: dehydration: with the distillation 1 hour under the condition of 20 ℃ of vacuum 400mmHg, temperature of the fatty-acid ethyl ester of the 11 step gained,
The 14 step: molecular distillation: the fatty-acid ethyl ester of the 12 step gained is entered international advanced complete molecular distillation apparatus, control pressure is at 0.1Pa, 80 ℃ of temperature, decolouring flavor is handled, and produces purity greater than 2.5 kilograms of the products of 80% Alpha-ethyl linolenate.
Embodiment 2:
The first step: oil expression: 300 kilograms of perilla seeds, adopt mechanical cold pressing process to squeeze perilla oil,
Second step: filter: the solid impurity in the perilla oil is leached, get 100 kilograms of perilla oils,
The 3rd step: saponification: with 100 kilograms of perilla oils; 400 kilograms of deionized waters; in 10 kilograms of adding containers of enzyme catalyst (lipolase100L), stir and heating, the control temperature of charge is between 70 ℃; control material pH value is 7; reaction times, sample thief was analyzed acid number at 20 hours, and reaction finishes when acid number reaches 120～210mgKOH/g; the omnidistance logical nitrogen protection of this process
The 4th step: acidifying: be in the material after 90% sulfuric acid slowly adds the saponification of the 3rd step gained with concentration and stir; control material reaction temperature is at 95 ℃; when the pH value of material is stopping to add sulfuric acid less than 4 the time; when the pH value of material greater than 4 the time, continue slowly to add sulfuric acid, repeat aforesaid operations; when the pH value of material less than 4 keep 2 hours constant after; reaction finishes, the omnidistance logical nitrogen protection of this process
The 5th step: washing: the 4th step gained material was left standstill 6 hours, emit lower aqueous solution, get 70 kilograms in lipid acid; the deionized water that in lipid acid, adds 280 kilograms; stir, left standstill 6 hours, emit lower aqueous solution again; repeat aforesaid operations; until the lower aqueous solution pH value of emitting is 7, and upper strata lipid acid enters next procedure, this end of processing; the omnidistance logical nitrogen protection of this process
The 6th step: urea complexation: 68 kilograms in the lipid acid of the 5th step output, 544 kilograms of adding containers of 544 kilograms of edible ethanols, urea of 99.9% are stirred; controlled temperature is at 100 ℃; 8 hours hold-times; then material is cooled to 60 ℃; this operation finishes; the omnidistance logical nitrogen protection of this operation
The 7th step: freezing: the material in the 6th step is carried out the stage cooling, and the fs is reduced to 0 ℃ from original temperature, and subordinate phase is reduced to-10 ℃ from 0 ℃; phase III is reduced to-20 ℃ from-10 ℃; the quadravalence section is reduced to-30 ℃ from-20 ℃, and five-stage is reduced to-40 ℃ from-30 ℃, and the 6th stage was reduced to-50 ℃ from-40 ℃; per stage insulation 8 hours; the uninterrupted stirring, when temperature reached requirement, this operation finished; the omnidistance logical nitrogen protection of this operation
The 8th step: press filtration: the 7th step gained material is realized solid-liquid separation with pressure and filtering net under-50 ℃ of states, get 500 kilograms of liquid materials, liquid material enters next procedure,
The 9th step: heat up: the material of the 8th step gained is warming up to 30 ℃, the omnidistance nitrogen protection of this operation,
The tenth goes on foot: extraction: the material and the deionized water of the 9th step gained are mixed and stir for 2000 kilograms, and standing demix is emitted lower aqueous solution, and get upper strata lipid acid and enter next procedure for 11 kilograms, the omnidistance nitrogen protection of this operation,
The 11 step: esterification: 11 kilograms in the lipid acid of the tenth step gained, 99.9% 22 kilograms of edible ethanols, 98% sulfuric acid mixed for 1.1 kilograms add in the container, 100 ℃ of control reaction temperature, 20 hours time, emit lower floor's solution after the cooling, repeat aforesaid operations, analyze acid number less than 10mgKOH/g until upper strata fatty-acid ethyl ester sample thief, this operation finishes.Get the upper strata fatty-acid ethyl ester and enter next procedure for 11 kilograms.
The 12 step: washing: the fatty-acid ethyl ester of the 11 step gained is added 44 kilograms of mixing of deionized water, and standing demix is discharged lower layer of water; repeating aforesaid operations, is 7 until the lower layer of water pH value, and the upper strata fatty-acid ethyl ester enters next procedure; the omnidistance nitrogen protection of this operation
The 13 step: dehydration: with the distillation 4 hours under the condition of 80 ℃ of vacuum 700mmHg, temperature of the fatty-acid ethyl ester of the 12 step gained,
The 14 step: molecular distillation: the fatty-acid ethyl ester of the 13 step gained is entered international advanced complete molecular distillation apparatus, control pressure is between 5Pa, 150 ℃ of temperature, decolouring flavor is handled, and produces purity greater than 9 kilograms of 80% alpha-linolenic acid products.
Embodiment 3:
The first step: oil expression: 300 kilograms of perilla seeds, adopt mechanical cold pressing process to squeeze perilla oil,
Second step: filter: the solid impurity in the perilla oil is leached, get 100 kilograms of perilla oils,
The 3rd step: saponification: with 100 kilograms of perilla oils; in deionized water 120 kg, 8 kilograms of adding containers of enzyme catalyst (lipolase100L); stir and heating; the control temperature of charge is between 55 ℃, and control material pH value is 7, and the reaction times was at 12 hours; sample thief is analyzed acid number; reaction finishes when acid number reaches 120～210mgKOH/g, the omnidistance logical nitrogen protection of this process
The 4th step: acidifying: be in the material after 80% sulfuric acid slowly adds the saponification of the 3rd step gained with concentration and stir; control material reaction temperature is between 75 ℃; when the pH value of material is stopping to add sulfuric acid less than 4 the time; when the pH value of material greater than 4 the time, continue slowly to add sulfuric acid, repeat aforesaid operations; when the pH value of material less than 4 keep 2 hours constant after; reaction finishes, the omnidistance logical nitrogen protection of this process
The 5th step: washing: the 4th step gained material was left standstill 3 hours, emit lower aqueous solution, get 68 kilograms in upper strata lipid acid; the deionized water that adds 50 kilograms; stir, left standstill 5 hours, emit lower aqueous solution again; repeat aforesaid operations; until the lower aqueous solution pH value is 7, and upper strata lipid acid enters next procedure, this end of processing; the omnidistance logical nitrogen protection of this process
The 6th step: urea complexation: 65 kilograms in the lipid acid of the 5th step output, 150 kilograms of adding containers of 100 kilograms of edible ethanols, urea of 90% are stirred, and controlled temperature is at 90 ℃, 3 hours hold-times; then material is cooled to 55 ℃; this operation finishes, the omnidistance logical nitrogen protection of this operation
The 7th step: freezing: the material in the 6th step is carried out the stage cooling, and the fs is reduced to 0 ℃ from original temperature, and subordinate phase is reduced to-6 ℃ from 0 ℃; phase III is reduced to-18 ℃ from-6 ℃; the quadravalence section is reduced to 21 ℃ from-18 ℃, and five-stage is reduced to 33 ℃ from 21 ℃, and the 6th stage was reduced to 49 ℃ from 33 ℃; per stage insulation 2 hours; the uninterrupted stirring, when temperature reached requirement, this operation finished; the omnidistance logical nitrogen protection of this operation
The 8th step: press filtration: make the 7th step gained material realize solid-liquid separation with pressure and filtering net under-15 ℃ of states, get 90 kilograms of liquid materials, liquid material enters next procedure,
The 9th step: heat up: the material of the 8th step gained is warming up to 25 ℃, the omnidistance nitrogen protection of this operation,
The tenth goes on foot: extraction: the material of the 9th step gained is added 165 kilograms of mixing of deionized water and stirring for 90 kilograms, and standing demix is emitted lower aqueous solution, and get upper strata lipid acid and enter next procedure for 10 kilograms, the omnidistance nitrogen protection of this operation,
The 11 step: esterification: 10 kilograms in the lipid acid of the tenth step gained, 90% 10 kilograms of edible ethanols, 80% sulfuric acid mixed for 0.06 kilogram add in the container, 95 ℃ of control reaction temperature, 10 hours time, emit lower floor's solution after the cooling, repeat aforesaid operations, analyze acid number less than 10mgKOH/g until upper strata fatty-acid ethyl ester sample thief, this operation finishes.The upper strata fatty-acid ethyl ester enters next procedure for 10 kilograms.
The 12 step: washing: the fatty-acid ethyl ester of the 11 step gained is added 10 kilograms of mixing of deionized water for 10 kilograms, and standing demix is discharged lower layer of water; repeating aforesaid operations, is 7 until the lower layer of water pH value, and the upper strata fatty-acid ethyl ester enters next procedure; the omnidistance nitrogen protection of this operation
The 13 step: dehydration: with the distillation 2 hours under the condition of 65 ℃ of vacuum 550mmHg, temperature of the fatty-acid ethyl ester of the 12 step gained,
The 14 step: molecular distillation: the fatty-acid ethyl ester of the 13 step gained is entered international advanced complete molecular distillation apparatus, control pressure is at 2Pa, 100 ℃ of temperature, decolouring flavor is handled, and produces purity greater than 8.5 kilograms of the products of 80% Alpha-ethyl linolenate.
Claims (1)
1, a kind of purity is characterized in that: carry out according to following technology greater than the production technique of 80% Alpha-ethyl linolenate:
The first step: oil expression: adopt mechanical cold pressing process to squeeze perilla oil perilla seed,
Second step: filter: the solid impurity in the perilla oil is leached,
The 3rd step: saponification: the second step gained perilla oil and deionized water, enzyme catalyst (lipolase100L) are added in the container according to the ratio of weight ratio 1: 0.5～4: 0.01～0.1; stir and heating; the control temperature of charge is between 40 ℃～70 ℃; control material pH value is 7; reaction times was at 2～20 hours; the omnidistance logical nitrogen protection of this process
The 4th step: acidifying: be in the material after 10%～90% sulfuric acid slowly adds the saponification of the 3rd step gained with concentration and stir; control material reaction temperature is between 40 ℃～95 ℃; when the material pH value stops to add sulfuric acid less than 4 the time; when the material pH value greater than 4 the time, continue to add sulfuric acid, repeat aforesaid operations; when the material pH value less than 4 keep 2 hours constant after; reaction finishes, the omnidistance logical nitrogen protection of this process
The 5th step: washing: the 4th step gained material was left standstill 1～6 hour; emit lower aqueous solution, in remaining upper strata lipid acid, add 0.5～4 times deionized water, stir; left standstill 1～6 hour; emitting lower aqueous solution again, repeat aforesaid operations, is 7 until the lower aqueous solution pH value of emitting; upper strata lipid acid enters next procedure; this end of processing, the omnidistance logical nitrogen protection of this process
The 6th step: urea complexation: with the lipid acid of the 5th step gained, 85%～99.9% edible ethanol, urea by weight 1: (1～8): the ratio of (1～8) adds container and stirs; controlled temperature is between 60 ℃～100 ℃; 0.5～8 hour hold-time; then material is cooled to 20 ℃～60 ℃; this operation finishes; the omnidistance logical nitrogen protection of this operation
The 7th step: freezing: the material of the 6th step gained is carried out the stage cooling; fs is reduced to 0 ℃ from original temperature; subordinate phase is reduced to (5～-10 ℃) from 0 ℃; phase III is reduced to (10～-20 ℃) from (5～-10 ℃); the quadravalence section is reduced to (20～-30 ℃) from (10～-20 ℃); five-stage is reduced to (30～-40 ℃) from (20～-30 ℃); the 6th stage was reduced to (40～-50 ℃) from (30～-40 ℃); per stage need be incubated 0.5～8 hour; the uninterrupted stirring, when temperature reached requirement, this operation finished; the omnidistance logical nitrogen protection of this operation
The 8th step: press filtration: the material of the 7th step gained is realized solid-liquid separation with pressure and filtering net under 0 ℃～-50 ℃ states, liquid enters next procedure,
The 9th step: heat up: the 8th step gained material is warming up to 10 ℃～30 ℃, the omnidistance nitrogen protection of this operation,
The tenth goes on foot: extraction: with the material and deionized water 1: 0.5～4 the mixed and the stirring by weight of the 9th step gained, standing demix is emitted lower aqueous solution, and upper strata lipid acid enters next procedure, the omnidistance nitrogen protection of this operation,
The 11 step: esterification: with the lipid acid of the tenth step gained, 85%～99.9% edible ethanol, 50%～98% sulfuric acid by weight 1: (0.2～2): the mixed of (0.05～0.1) adds in the container, between 70 ℃～100 ℃ of the control reaction temperature, 4～20 hours time, emit lower floor's solution after the cooling, repeat aforesaid operations, analyze acid number less than 10mgKOH/g until upper strata fatty-acid ethyl ester sample thief, this operation finishes, the upper strata fatty-acid ethyl ester enters next procedure
The 12 step: washing: the 11 step fatty-acid ethyl ester of gained and the deionized water ratio by weight 1: 0.5～4 entered mix in the container; standing demix; discharge lower layer of water; repeat aforesaid operations; until the lower layer of water pH value is 7; the upper strata fatty-acid ethyl ester enters next procedure, the omnidistance nitrogen protection of this operation
The 13 step: dehydration: the fatty-acid ethyl ester of the 12 step gained was distilled 1～4 hour under the condition of 20 ℃～80 ℃ of vacuum 400～700mmHg, temperature,
The 14 step: molecular distillation: the fatty-acid ethyl ester of the 13 step gained is sent into complete molecular distillation apparatus, control pressure is between 0.1～5Pa, 80 ℃～150 ℃ of temperature, decolouring flavor is handled, and produces purity greater than 80% Alpha-ethyl linolenate product.
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| CN102559393A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for preparing biodiesel with low acid value |
| CN102993011A (en) * | 2011-09-13 | 2013-03-27 | 丰宁京北第一草原原生态食品科技开发有限公司 | Method for preparing alpha-ethyl linolenate through using Fructus Perillae oil |
| CN104693033A (en) * | 2014-09-28 | 2015-06-10 | 河南利诺生化有限责任公司 | Production process of high-purity alpha-ethyl linolenate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATE178582T1 (en) * | 1994-05-09 | 1999-04-15 | Nestle Sa | METHOD FOR PRODUCING A CONCENTRATE OF ESTERS OF POLYUNSATURATED FATTY ACIDS |
| CN1095824C (en) * | 2000-04-13 | 2002-12-11 | 胡德甫 | Process for preparing high-purity alpha-linolenic acid |
| CN1394944A (en) * | 2001-07-11 | 2003-02-05 | 北京万博力科技发展有限公司 | Method for preparing alpha-ethyl linolenate from linseed oil by means of ester exchange |
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- 2005-12-30 CN CNB2005101073551A patent/CN100366601C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102559393A (en) * | 2010-12-23 | 2012-07-11 | 中国石油化工股份有限公司 | Method for preparing biodiesel with low acid value |
| CN102993011A (en) * | 2011-09-13 | 2013-03-27 | 丰宁京北第一草原原生态食品科技开发有限公司 | Method for preparing alpha-ethyl linolenate through using Fructus Perillae oil |
| CN102993011B (en) * | 2011-09-13 | 2015-01-14 | 丰宁京北第一草原原生态食品科技开发有限公司 | Method for preparing alpha-ethyl linolenate through using Fructus Perillae oil |
| CN104693033A (en) * | 2014-09-28 | 2015-06-10 | 河南利诺生化有限责任公司 | Production process of high-purity alpha-ethyl linolenate |
| CN104693033B (en) * | 2014-09-28 | 2016-08-31 | 河南利诺生化有限责任公司 | The production technology of highly purified a-ethyl linolenate |
| CN107459456A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of method that methyl stearate is extracted in the benzoyl methane raffinate from stearic acid |
| CN106281723A (en) * | 2016-08-31 | 2017-01-04 | 菏泽尧舜牡丹生物科技有限公司 | A kind of high ethyl esterified technique of acid value peony seed oil |
| CN112479885A (en) * | 2021-01-01 | 2021-03-12 | 河南利诺生化有限责任公司 | Low-cost environment-friendly production process of ethyl linolenate |
| CN112479885B (en) * | 2021-01-01 | 2023-04-14 | 河南利诺生化有限责任公司 | Low-cost environment-friendly production process of ethyl linolenate |
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Assignee: He'nan Linuo Bio-chemistry Co., Ltd. Assignor: Anyang Chemical Industry Group Co., Ltd. Contract record no.: 2010410000157 Denomination of invention: Process for producing alpha linolenic acid ethyl ester with purity greater than 80% Granted publication date: 20080206 License type: Exclusive License Open date: 20060927 Record date: 20101116 |
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