CN1560015A - Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil - Google Patents
Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil Download PDFInfo
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- CN1560015A CN1560015A CNA2004100164987A CN200410016498A CN1560015A CN 1560015 A CN1560015 A CN 1560015A CN A2004100164987 A CNA2004100164987 A CN A2004100164987A CN 200410016498 A CN200410016498 A CN 200410016498A CN 1560015 A CN1560015 A CN 1560015A
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- acid
- linoleic acid
- conjugated diene
- oleum gossypii
- gossypii semen
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Abstract
The invention discloses a technique of producing conjugated alkadiene linoleic acid and palmitic acid by cotton seed oil, selecting cotton seed oil as raw material to make isomerization, acidification, salt wash, water wash, freezing and separation so as to obtain the palmitic acid, and then enveloping and purifying the separated liquid fatty acid to obtain conjugated alkadiene linoleic acid. It can obtain the conjugated alkadiene linoleic acid with purity higher than 90% and colourity Gardner less than 2, and the palmitic acid with purity higher than 90%, and can largely increase technological added value of cotton seed oil.
Description
Technical field
The present invention relates to a kind of technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen.
Background technology
Conjugated diene-linoleic acid is a series of linolic acid general names that contain conjugated double bond, conjugated diene-linoleic acid mainly is present in the butterfat and meat product of ruminating animal ox, sheep etc. at nature, in some plants, also found the existence of conjugated diene-linoleic acid, but content is few.Conjugated diene-linoleic acid has special physiological properties, has effects such as antitumous effect, atherosclerosis, reducing blood-fat, strengthening immunity and fat-reducing, can be widely used in fields such as medicine, food and feed.Palmitinic acid [CH
3(CH
2)
14COOH] be mainly used in products such as producing alcohol, amine, acid amides and sulfonation, be widely used in daily chemical products, medicine, plastics, weaving, leather industry.Cotton is a main farm produce in the world, and its Oleum Gossypii semen belongs to the row of high linoleic acid, also belongs to the row of high palmitinic acid simultaneously, and palmitinic acid accounts for 20-23% in its fat, and linolic acid accounts for 45-59%.Oleum Gossypii semen is mainly used in edible now, and linolic acid, palmitinic acid height can make full use of in its grease, also is easy to purify.
Summary of the invention
Purpose of the present invention just provides a kind of scientific and technological added value that can increase Oleum Gossypii semen, is produced the technology of conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen.
A kind of technology by Oleum Gossypii semen production conjugated diene-linoleic acid, palmitinic acid of the present invention is: put into solvent, alkali with Oleum Gossypii semen; under protection of inert gas; carry out isomerization reaction; through cooling, acidifying, salt wash, wash, dehydration, subzero fractionation; separate the back solid phase and obtain palmitinic acid through washing, drying; isolating liquid fatty acid joins and carries out envelope in the ethanol urea soln, filters, reclaims ethanol, washes, is drying to obtain conjugated diene-linoleic acid.Described solvent is 1, and 2-propylene glycol, alkali are KOH or NaOH, and rare gas element is N
2, used tensio-active agent " 601 " and sal epsom during subzero fractionation.The subzero fractionation temperature is controlled at 0-10 ℃; Lipid acid is 1 with the urea quality ratio: 0.65-0.75, urea and ethanol mass ratio are 1: 1.8-2.6.
In a kind of technology of the present invention, generate water-soluble gossypol sodium salt, can remove remaining AFB in the Oleum Gossypii semen with gossypol in alkali KOH or NaOH and the Oleum Gossypii semen and derivative effect thereof by Oleum Gossypii semen production conjugated diene-linoleic acid, palmitinic acid
1And pigment, make product conjugated diene-linoleic acid color and luster Gardner less than 2, this technology can prepare purity greater than 90% conjugated diene-linoleic acid and purity greater than 90% palmitinic acid, can improve the scientific and technological added value of Oleum Gossypii semen greatly.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Embodiment: a kind of technology by Oleum Gossypii semen production conjugated diene-linoleic acid, palmitinic acid is:
1, isomerization: with 80g1,2-propylene glycol and 15g potassium hydroxide mix, and pour nitrogen, and heating for dissolving stirs, and opens water of condensation, continues to be heated to 160 ℃, adds the 50g Oleum Gossypii semen, and constant temperature reacted 2.5 hours under nitrogen protection for 160 ℃.Reactant is cooled to 40 ℃, stirs, add the 4N hydrochloric acid soln to pH value less than 2.Left standstill 30 minutes, and bled off lower floor's waste liquid of standing demix solution.With the material of retaining, add the 100ml3% salt solution, washing is left standstill, and bleeds off lower floor's waste liquid, so repeats two to three times; Add 100g hot water, washing is left standstill, and bleeds off lower floor's waste liquid, repeats two to three times again, and the pH value that is washed till washing water is till 6-7.To wash good oil phase material under 90 ℃, vacuum hydro-extraction 30 minutes.
2, subzero fractionation: above-mentioned oil phase stirring was cooled to 5 ℃, 8 hours, stirs the tensio-active agent " 601 " of adding 6.5% and 3% magnesium sulfate solution, 150% cold water (water temperature is identical with the material temperature) is centrifugated into the weight two-phase.Heavy phase is the aqueous solution of palmitinic acid and tensio-active agent " 601 ", is heated to 90 ℃, and standing demix is told the upper strata palmitinic acid, washes three times, and under 90 ℃, vacuum hydro-extraction obtained palmitinic acid in 30 minutes.Gently be heated to 90 ℃ mutually earlier, it is inferior to give a baby a bath on the third day after its birth with 90 ℃ of hot water, under 90 ℃, and vacuum hydro-extraction 30 minutes, it is stand-by to obtain thick conjugated diene-linoleic acid.
3, urea clathrate is purified: is 1: 0.72 by thick conjugated diene-linoleic acid with the urea quality ratio; Urea is 1: 2.1 batching with the ethanol ratio.The ethanol and the urea that prepare material are mixed stirring, heating, ethanol is obviously refluxed, the urea dissolution process is controlled at 83 ℃, 2 hours time, treat urea dissolving after, in 20 minutes, add thick conjugated diene-linoleic acid, be cooled to 63 ℃, reacted 3 hours, left standstill 8 hours, press filtration, liquid phase boils off ethanol (recovery ethanol), leaves standstill under the room temperature 8 hours, filters, liquid phase is with 90 ℃ of hot washes four times, to PH be 6-7, under 90 ℃, vacuum hydro-extraction obtained in 30 minutes purity greater than 90%, the conjugated diene-linoleic acid of lighter color (Gardner is less than 2).
Claims (6)
1, a kind of technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen; it is characterized in that: put into solvent, alkali with Oleum Gossypii semen; under protection of inert gas; carry out isomerization reaction; through cooling, acidifying, salt wash, wash, dehydration, subzero fractionation; separate the back solid phase and obtain palmitinic acid through washing, drying, isolating liquid fatty acid joins and carries out envelope in the ethanol urea soln, filters, reclaims ethanol, washes, is drying to obtain conjugated diene-linoleic acid.
2, according to right 1 described technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen, it is characterized in that: described solvent is 1, the 2-propylene glycol.
3, according to right 1 described technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen, it is characterized in that: described alkali is KOH or NaOH.
4, according to right 1 described technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen, it is characterized in that: described rare gas element is a nitrogen.
5, according to right 1 described technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen, it is characterized in that: the subzero fractionation temperature is controlled at 0-10 ℃, uses tensio-active agent " 601 " and sal epsom.
6, according to right 1 described technology of producing conjugated diene-linoleic acid, palmitinic acid by Oleum Gossypii semen, it is characterized in that: urea and ethanol mass ratio are 1 in the described ethanol urea soln: 1.8-2.6, lipid acid is 1 with the urea quality ratio: 0.65-0.75.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100164987A CN1560015A (en) | 2004-02-20 | 2004-02-20 | Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100164987A CN1560015A (en) | 2004-02-20 | 2004-02-20 | Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1560015A true CN1560015A (en) | 2005-01-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2004100164987A Pending CN1560015A (en) | 2004-02-20 | 2004-02-20 | Process for producing conjugated diolefine linoleic acid, palmic acid by cotton seed oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408660C (en) * | 2006-07-07 | 2008-08-06 | 白长军 | Method of extracting cotton seed oil |
| CN106946684A (en) * | 2017-03-01 | 2017-07-14 | 余海龙 | It is a kind of to refine the method that accessory substance prepares CLA using small rice germ oil |
| CN108569963A (en) * | 2018-05-02 | 2018-09-25 | 广东广益科技实业有限公司 | A kind of production technology of palmitic acid waste residue recycling |
| CN110305488A (en) * | 2019-07-08 | 2019-10-08 | 广州正浩新材料科技有限公司 | A kind of aqueous ethylene bis stearic acid amide lotion and preparation method thereof |
-
2004
- 2004-02-20 CN CNA2004100164987A patent/CN1560015A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408660C (en) * | 2006-07-07 | 2008-08-06 | 白长军 | Method of extracting cotton seed oil |
| CN106946684A (en) * | 2017-03-01 | 2017-07-14 | 余海龙 | It is a kind of to refine the method that accessory substance prepares CLA using small rice germ oil |
| CN106946684B (en) * | 2017-03-01 | 2019-11-08 | 余海龙 | A method of conjugated linoleic acid is prepared using small rice germ oil refining by-product |
| CN108569963A (en) * | 2018-05-02 | 2018-09-25 | 广东广益科技实业有限公司 | A kind of production technology of palmitic acid waste residue recycling |
| CN110305488A (en) * | 2019-07-08 | 2019-10-08 | 广州正浩新材料科技有限公司 | A kind of aqueous ethylene bis stearic acid amide lotion and preparation method thereof |
| CN110305488B (en) * | 2019-07-08 | 2021-08-31 | 广州正浩新材料科技有限公司 | Water-based ethylene bis stearamide emulsion and preparation method thereof |
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