CN107325144B - The extracting method of cholesterol in a kind of lanolin - Google Patents
The extracting method of cholesterol in a kind of lanolin Download PDFInfo
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- CN107325144B CN107325144B CN201710518900.9A CN201710518900A CN107325144B CN 107325144 B CN107325144 B CN 107325144B CN 201710518900 A CN201710518900 A CN 201710518900A CN 107325144 B CN107325144 B CN 107325144B
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- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
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Abstract
The invention discloses a kind of extracting methods of cholesterol in lanolin comprising pretreatment, saponification, extraction, condensing crystallizing, dissolving crystallized, recrystallization, drying and other steps.Acrylic acid -2- acrylamide-2-methyl propane sulfonic copolymer and sodium gluconate will be added in pre-treatment step of the present invention in lanolin after acidification, after isothermal reaction and impulse electric field processing, effectively impurity can be separated from the cholesterol in lanolin, to improve the purity of cholesterol；The present invention carries out continuous extraction using alkanes reagent, the extraction yield of cholesterol can be significantly improved, to improve the yield of cholesterol.The cholesterol yield that extracting method of the present invention obtains is 95% or more, and purity is 98% or more, and process stabilizing, is easy to industrialize.
Description
Technical field
The present invention relates to a kind of extracting methods of cholesterol, and in particular to the extracting method of cholesterol in a kind of lanolin.
Background technique
Cholesterol is also referred to as cholesterine, is the indispensable important substance of animal tissue cell, and with industrial use
Natural materials, there is the extensive market demand, are industrially mainly used for cosmetics, emulsifier, medicine etc..Cholesterol both can be driven
It extracts, and can be extracted from lanolin in object brain tissue and myeloid tissue.Preceding kind of method is unable to satisfy since its resource is limited
Growing demand.Not only there is higher cholesterol level in lanolin, but also from a wealth of sources in China, discharge amount is big, can
As the main source of cholesterol, therefore how cholesterol to be separated from lanolin just as key technology.However mesh
The shortcomings that mostly there is yields is low for the preceding method that cholesterol is extracted from lanolin, purity difference, is unable to satisfy the demand in market.
Summary of the invention
It, should it is an object of the invention in view of the shortcomings of the prior art, provide a kind of extracting method of cholesterol in lanolin
The cholesterol yield that method obtains is 95% or more, and purity is 98% or more, and process stabilizing, is easy to industrialize.
To achieve the above object, the present invention adopts the following technical scheme that:
The extracting method of cholesterol in a kind of lanolin, it is to prepare according to the following steps:
(1) it pre-processes: lanolin is heated to 40-45 DEG C, be added after lanolin all fusing and be equivalent to wool lipid
The dilution heat of sulfuric acid of 8-10% is measured, 40-50min, standing sedimentation 25-35min are stirred, releases leftover bits and pieces, after cleaning acidification with hot water
Lanolin 2-3 times, until the leftover bits and pieces pH that is discharged is in neutrality；Lanolin after acidification is heated to 40-45 DEG C, wait be acidified
Acrylic acid -2- acrylamide -2- the first of the lanolin quality 5-8% after being equivalent to acidification is added in lanolin afterwards after all melting
The sodium gluconate of base sulphonic acid copolymer and 3-6%, insulation reaction 2-4h, is then cleaned 2-3 times with hot water, after cleaning
Lanolin impulse electric field under conditions of electric field strength is 20-40kV/cm, impulse electric field frequency is 400-600Hz handles 3-5s,
20-30min is stood, lower layer's dark brown liquid impurity is then slowly released, upper layer lanolin is cleaned 2-3 times with hot water；
(2) it is saponified: weighing step (1) pretreated lanolin, be then added and be equivalent to lanolin quality 0.2-0.4
Potassium hydroxide, 0.6-0.8 times of purified water and 1.5-2 times of lower alcohol again is heated to reflux and starts timing, saponification
1.5-2h is cooled to 30-40 DEG C；
(3) it extracts: the purified water for being equivalent to 0.8-1 times of saponification liquor quality being added into saponification liquor made from step (2), use
Then the alkanes reagent for being equivalent to 5-6 times of saponification liquor quality is added in dilute sulfuric acid tune pH to 7-9, stir 10-15min, stands 1-
2h divides and removes saponification liquid layer, continues to add alkanes reagent to saponification liquid layer, repeats the above steps 3-5 times, merge alkanes reagent
Layer；
(4) condensing crystallizing: the alkanes reagent layer that step (3) merge is concentrated to dryness, and addition is equivalent to above-mentioned dense
The volume fraction of 6-8 times of contracting product quality is the ethanol solution of 90-95%, 60-70 DEG C of heating water bath, is stirred complete to enriched product
With dilute sulfuric acid tune pH to 1-3 after fully dissolved, reflux 30-60min being reheated, is filtered while hot, collects filtrate, cooling down crystallizes,
Crystal is collected by filtration；
(5) dissolving crystallized: to be added into crystal made from step (4) and be equivalent to 6-8 times of crystal quality of volume fraction and be
The ethanol solution of 95-97% adds the hydrogen peroxide for being equivalent to solution quality 0.5-1%, is stirred to react after dilute sulfuric acid tune pH to 4-6
After 30-60min, it is heated to reflux 1-2h, is filtered, filtrate is collected, cooling down crystallizes 8-10h, filters up to crude product cholesterol；
(6) recrystallize: it is 97- that into crude product cholesterol, addition, which is equivalent to 8-10 times of quality of crude product cholesterol of volume fraction,
100% ethanol solution, and pH to 9-10 is adjusted, it is heated to reflux 1-2h, cooling down crystallization is filtered up to fine work cholesterol；
(7) it dries: fine work cholesterol being put into drying box and is dried, set drying temperature as 50-60 DEG C, dry 1-
2h, resetting drying temperature is 70-90 DEG C, and dry 2-3h is to get fine work cholesterol finished product.
The concentration of dilute sulfuric acid described in step (1) is 45-50%
Lower alcohol described in step (2) is that one of methanol, ethyl alcohol or the two mix.
Alkanes reagent described in step (3) is that one of n-hexane, hexamethylene, heptane, octane or the two mix.
The concentration of dilute sulfuric acid described in step (3), step (4) and step (5) is 5-20%.
Beneficial effects of the present invention:
Acrylic acid -2- acrylamide -2- methyl-prop sulphur will be added in pre-treatment step of the present invention in lanolin after acidification
Acid copolymer and sodium gluconate can be effectively by impurity from the gallbladders in lanolin after isothermal reaction and impulse electric field processing
Sterol is separated, to improve the purity of cholesterol；The present invention carries out continuous extraction using alkanes reagent, can significantly mention
The extraction yield of high cholesterol, to improve the yield of cholesterol.The cholesterol yield that extracting method of the present invention obtains 95% with
On, purity is 98% or more, and process stabilizing, is easy to industrialize.
Specific embodiment
Embodiment 1
The extracting method of cholesterol in a kind of lanolin, it is to prepare according to the following steps:
(1) it pre-processes: lanolin is heated to 40 DEG C, be added after lanolin all fusing and be equivalent to lanolin quality 8%
Dilution heat of sulfuric acid, stir 40min, standing sedimentation 25min, release leftover bits and pieces, with hot water clean be acidified after lanolin 2 times,
Until the leftover bits and pieces pH discharged is in neutrality；Lanolin after acidification is heated to 40 DEG C, the lanolin after being acidified is all molten
Acrylic acid -2- acrylamide-2-methyl propane sulfonic the copolymer and 3% of the lanolin quality 5% after being equivalent to acidification is added after change
Sodium gluconate, then insulation reaction 4h cleans 2 times with hot water, in electric field strength be 20kV/ by the lanolin after cleaning
Impulse electric field handles 5s under conditions of cm, impulse electric field frequency are 400Hz, stands 20min, then slowly releases lower layer's dark brown
Liquid impurity, upper layer lanolin are cleaned 2 times with hot water；
(2) it is saponified: weighing step (1) pretreated lanolin, be then added and be equivalent to 0.2 times of lanolin quality
Potassium hydroxide, 0.6 times of purified water and 1.5 times of lower alcohol are heated to reflux and start timing, be saponified 1.5h, be cooled to
30℃；
(3) extract: into saponification liquor made from step (2), addition is equivalent to 0.8 times of saponification liquor quality of purified water, and use is dilute
Sulfuric acid tune pH to 7, then addition is equivalent to 5 times of saponification liquor quality of alkanes reagent, stirs 10min, stands 1h, divides and goes to be saponified
Liquid layer continues to add alkanes reagent to saponification liquid layer, repeats the above steps 3 times, merge alkanes reagent layer；
(4) condensing crystallizing: the alkanes reagent layer that step (3) merge is concentrated to dryness, and addition is equivalent to above-mentioned dense
The ethanol solution that the volume fraction that 6 times of contracting product quality is 90%, 60 DEG C of heating water bath, after stirring is completely dissolved to enriched product
With dilute sulfuric acid tune pH to 1, reflux 30min is reheated, is filtered while hot, collect filtrate, crystal is collected by filtration in cooling down crystallization；
(5) dissolving crystallized: it is 95% that into crystal made from step (4), addition, which is equivalent to 6 times of crystal quality of volume fraction,
Ethanol solution add the hydrogen peroxide for being equivalent to solution quality 0.5%, after being stirred to react 30min, add after dilute sulfuric acid tune pH to 4
Filtrate is collected in heat reflux 1h, filtering, and cooling down crystallizes 8h, is filtered up to crude product cholesterol；
(6) recrystallize: being added into crude product cholesterol and being equivalent to the volume fraction of 8 times of crude product cholesterol quality is 97%
Ethanol solution, and pH to 9 is adjusted, it is heated to reflux 1h, cooling down crystallization is filtered up to fine work cholesterol；
(7) it dries: fine work cholesterol being put into drying box and is dried, set drying temperature as 50 DEG C, dry 2h, then
Drying temperature is set as 70 DEG C, dry 3h is to get fine work cholesterol finished product.
The concentration of dilute sulfuric acid described in step (1) is 45%
Lower alcohol described in step (2) is methanol.
Alkanes reagent described in step (3) is n-hexane.
The concentration of dilute sulfuric acid described in step (3), step (4) and step (5) is 5%.
The yield of above-described embodiment cholesterol is 95.23%, purity 98.15%.
Embodiment 2
The extracting method of cholesterol in a kind of lanolin, it is to prepare according to the following steps:
(1) it pre-processes: lanolin is heated to 42 DEG C, be added after lanolin all fusing and be equivalent to lanolin quality 9%
Dilution heat of sulfuric acid, stir 45min, standing sedimentation 30min, release leftover bits and pieces, with hot water clean be acidified after lanolin 3 times,
Until the leftover bits and pieces pH discharged is in neutrality；Lanolin after acidification is heated to 42 DEG C, the lanolin after being acidified is all molten
Acrylic acid -2- acrylamide-2-methyl propane sulfonic the copolymer and 4% of the lanolin quality 6% after being equivalent to acidification is added after change
Sodium gluconate, then insulation reaction 3h cleans 3 times with hot water, in electric field strength be 30kV/ by the lanolin after cleaning
Impulse electric field handles 4s under conditions of cm, impulse electric field frequency are 500Hz, stands 25min, then slowly releases lower layer's dark brown
Liquid impurity, upper layer lanolin are cleaned 3 times with hot water；
(2) it is saponified: weighing step (1) pretreated lanolin, be then added and be equivalent to 0.3 times of lanolin quality
Potassium hydroxide, 0.7 times of purified water and 1.8 times of lower alcohol are heated to reflux and start timing, be saponified 1.8h, be cooled to
35℃；
(3) extract: into saponification liquor made from step (2), addition is equivalent to 0.9 times of saponification liquor quality of purified water, and use is dilute
Sulfuric acid tune pH to 8, then addition is equivalent to 5.5 times of saponification liquor quality of alkanes reagent, stirs 12min, stands 1.5h, divides and goes
It is saponified liquid layer, continues to add alkanes reagent to saponification liquid layer, repeats the above steps 4 times, merge alkanes reagent layer；
(4) condensing crystallizing: the alkanes reagent layer that step (3) merge is concentrated to dryness, and addition is equivalent to above-mentioned dense
The ethanol solution that the volume fraction that 7 times of contracting product quality is 92%, 65 DEG C of heating water bath, after stirring is completely dissolved to enriched product
With dilute sulfuric acid tune pH to 2, reflux 45min is reheated, is filtered while hot, collect filtrate, crystal is collected by filtration in cooling down crystallization；
(5) dissolving crystallized: it is 96% that into crystal made from step (4), addition, which is equivalent to 7 times of crystal quality of volume fraction,
Ethanol solution add the hydrogen peroxide for being equivalent to solution quality 0.8%, after being stirred to react 45min, add after dilute sulfuric acid tune pH to 5
Filtrate is collected in heat reflux 1.5h, filtering, and cooling down crystallizes 9h, is filtered up to crude product cholesterol；
(6) recrystallize: being added into crude product cholesterol and being equivalent to the volume fraction of 9 times of crude product cholesterol quality is 98%
Ethanol solution, and pH to 9.5 is adjusted, it is heated to reflux 1.5h, cooling down crystallization is filtered up to fine work cholesterol；
(7) it dries: fine work cholesterol being put into drying box and is dried, set drying temperature as 55 DEG C, dry 1.5h,
Resetting drying temperature is 80 DEG C, and dry 2.5h is to get fine work cholesterol finished product.
The concentration of dilute sulfuric acid described in step (1) is 48%
Lower alcohol described in step (2) is methanol, ethyl alcohol is mixed according to isometric ratio.
Alkanes reagent described in step (3) is hexamethylene, heptane is mixed according to isometric ratio.
The concentration of dilute sulfuric acid described in step (3), step (4) and step (5) is 15%.
The yield of above-described embodiment cholesterol is 95.95%, purity 98.88%.
Embodiment 3
The extracting method of cholesterol in a kind of lanolin, it is to prepare according to the following steps:
(1) it pre-processes: lanolin is heated to 45 DEG C, be added after lanolin all fusing and be equivalent to lanolin quality
10% dilution heat of sulfuric acid stirs 50min, standing sedimentation 35min, releases leftover bits and pieces, the lanolin 3 after cleaning acidification with hot water
It is secondary, until the leftover bits and pieces pH discharged is in neutrality；Lanolin after acidification is heated to 45 DEG C, the lanolin after being acidified is whole
After fusing be added be equivalent to acidification after lanolin quality 8% acrylic acid -2- acrylamide-2-methyl propane sulfonic copolymer and
Then 6% sodium gluconate, insulation reaction 4h are cleaned 3 times with hot water, by the lanolin after cleaning electric field strength be 40kV/
Impulse electric field handles 3s under conditions of cm, impulse electric field frequency are 600Hz, stands 30min, then slowly releases lower layer's dark brown
Liquid impurity, upper layer lanolin are cleaned 3 times with hot water；
(2) it is saponified: weighing step (1) pretreated lanolin, be then added and be equivalent to 0.4 times of lanolin quality
Potassium hydroxide, 0.8 times of purified water and 2 times of lower alcohol are heated to reflux and start timing, be saponified 2h, be cooled to 40 DEG C；
(3) extract: into saponification liquor made from step (2), addition is equivalent to 1 times of saponification liquor quality of purified water, with dilute sulphur
Sour to adjust pH to 9, then addition is equivalent to 6 times of saponification liquor quality of alkanes reagent, stirs 15min, stands 2h, divides and removes saponification liquor
Layer continues to add alkanes reagent to saponification liquid layer, repeats the above steps 5 times, merge alkanes reagent layer；
(4) condensing crystallizing: the alkanes reagent layer that step (3) merge is concentrated to dryness, and addition is equivalent to above-mentioned dense
The ethanol solution that the volume fraction that 8 times of contracting product quality is 95%, 70 DEG C of heating water bath, after stirring is completely dissolved to enriched product
With dilute sulfuric acid tune pH to 3, reflux 60min is reheated, is filtered while hot, collect filtrate, crystal is collected by filtration in cooling down crystallization；
(5) dissolving crystallized: it is 97% that into crystal made from step (4), addition, which is equivalent to 8 times of crystal quality of volume fraction,
Ethanol solution add the hydrogen peroxide for being equivalent to solution quality 1% after dilute sulfuric acid tune pH to 6, after being stirred to react 60min, heating
Flow back 2h, filtering, collects filtrate, and cooling down crystallizes 10h, filters up to crude product cholesterol；
(6) recrystallize: being added into crude product cholesterol and being equivalent to the volume fraction of 10 times of crude product cholesterol quality is 100%
Ethanol solution, and adjust pH to 10, be heated to reflux 2h, cooling down crystallization is filtered up to fine work cholesterol；
(7) it dries: fine work cholesterol being put into drying box and is dried, set drying temperature as 60 DEG C, dry 1h, then
Drying temperature is set as 90 DEG C, dry 2h is to get fine work cholesterol finished product.
The concentration of dilute sulfuric acid described in step (1) is 50%
Lower alcohol described in step (2) is ethyl alcohol.
Alkanes reagent described in step (3) is octane.
The concentration of dilute sulfuric acid described in step (3), step (4) and step (5) is 20%.
The yield of above-described embodiment cholesterol is 95.84%, purity 98.33%.
Claims (4)
1. the extracting method of cholesterol in a kind of lanolin, it is characterised in that: it is to prepare according to the following steps:
(1) it pre-processes: lanolin is heated to 40-45 DEG C, be added after lanolin all fusing and be equivalent to lanolin quality 8-
10% dilution heat of sulfuric acid stirs 40-50min, standing sedimentation 25-35min, releases leftover bits and pieces, the sheep after cleaning acidification with hot water
Hair rouge 2-3 times, until the leftover bits and pieces pH discharged is in neutrality；Lanolin after acidification is heated to 40-45 DEG C, after being acidified
Acrylic acid -2- acrylamide -2- the methyl-prop of the lanolin quality 5-8% after being equivalent to acidification is added in lanolin after all melting
The sodium gluconate of sulfonic acid copolymer and 3-6%, insulation reaction 2-4h, is then cleaned 2-3 times with hot water, by the wool after cleaning
Rouge impulse electric field under conditions of electric field strength is 20-40kV/cm, impulse electric field frequency is 400-600Hz handles 3-5s, stands
20-30min, then slowly releases lower layer's dark brown liquid impurity, and upper layer lanolin is cleaned 2-3 times with hot water；
(2) it is saponified: weighing step (1) pretreated lanolin, be then added and be equivalent to 0.2-0.4 times of lanolin quality
Potassium hydroxide, 0.6-0.8 times of purified water and 1.5-2 times of lower alcohol are heated to reflux and start timing, be saponified 1.5-
2h is cooled to 30-40 DEG C；
(3) it extracts: the purified water for being equivalent to 0.8-1 times of saponification liquor quality being added into saponification liquor made from step (2), with dilute sulphur
Acid adjusts pH to 7-9, and the alkanes reagent for being equivalent to 5-6 times of saponification liquor quality is then added, and stirs 10-15min, stands 1-2h,
Divide and remove saponification liquid layer, continues to add alkanes reagent to saponification liquid layer, repeat the above steps 3-5 times, merge alkanes reagent layer, institute
The alkanes reagent stated is that one of n-hexane, hexamethylene, heptane, octane or the two mix；
(4) condensing crystallizing: the alkanes reagent layer that step (3) merge is concentrated to dryness, and addition is equivalent to above-mentioned concentration and produces
6-8 times of amount of substance of volume fraction is the ethanol solution of 90-95%, heats 60-70 DEG C, after stirring is completely dissolved to enriched product
With dilute sulfuric acid tune pH to 1-3, reflux 30-60min is reheated, is filtered while hot, collect filtrate, cooling down crystallization is collected by filtration
Crystal；
(5) dissolving crystallized: it is 95- that into crystal made from step (4), addition, which is equivalent to 6-8 times of crystal quality of volume fraction,
97% ethanol solution adds the hydrogen peroxide for being equivalent to solution quality 0.5-1%, is stirred to react 30- after dilute sulfuric acid tune pH to 4-6
After 60min, it is heated to reflux 1-2h, is filtered, filtrate is collected, cooling down crystallizes 8-10h, filters up to crude product cholesterol；
(6) recrystallize: it is 97-100% that into crude product cholesterol, addition, which is equivalent to 8-10 times of quality of crude product cholesterol of volume fraction,
Ethanol solution, and adjust pH to 9-10, be heated to reflux 1-2h, cooling down crystallization is filtered up to fine work cholesterol；
(7) it dries: fine work cholesterol being put into drying box and is dried, set drying temperature as 50-60 DEG C, dry 1-2h,
Resetting drying temperature is 70-90 DEG C, and dry 2-3h is to get fine work cholesterol finished product.
2. the extracting method of cholesterol in a kind of lanolin according to claim 1, it is characterised in that: step (1) is described
Dilute sulfuric acid concentration be 45-50%.
3. the extracting method of cholesterol in a kind of lanolin according to claim 1, it is characterised in that: step (2) is described
Lower alcohol be that one of methanol, ethyl alcohol or the two mix.
4. the extracting method of cholesterol in a kind of lanolin according to claim 1, it is characterised in that: step (3), step
(4) and the concentration of dilute sulfuric acid described in step (5) is 5-20%.
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| CN103102380A (en) * | 2013-02-25 | 2013-05-15 | 上海艾韦特医药科技有限公司 | Production method of high purity lanolin cholesterol |
| CN103113446A (en) * | 2013-03-15 | 2013-05-22 | 北京化工大学 | Method for separating and extracting sterol from wool fat |
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| CN103102380A (en) * | 2013-02-25 | 2013-05-15 | 上海艾韦特医药科技有限公司 | Production method of high purity lanolin cholesterol |
| CN103113446A (en) * | 2013-03-15 | 2013-05-22 | 北京化工大学 | Method for separating and extracting sterol from wool fat |
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