CN108840795A - A method of lanolin fatty acid and lanonol are prepared by lanolin - Google Patents
A method of lanolin fatty acid and lanonol are prepared by lanolin Download PDFInfo
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- CN108840795A CN108840795A CN201810895421.3A CN201810895421A CN108840795A CN 108840795 A CN108840795 A CN 108840795A CN 201810895421 A CN201810895421 A CN 201810895421A CN 108840795 A CN108840795 A CN 108840795A
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- lanolin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- 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 methods for preparing lanolin fatty acid and lanonol by lanolin, including, the saponification mixture obtained after lanolin is saponified, by obtaining the mixture of lanolin fatty acid calcium and fatty alcohol after the progress calcification of excess chlorination calcium solution in hydrochloric acid and after remaining alkaline reagent, is added；Then alcohol is washed to obtain lanonol, lanolin fatty acid calcium under conditions of 55~80 DEG C；The lanolin fatty acid calcium that alcohol obtains after washing obtains crude lanolin fatty acid after pickling, then the crude lanolin fatty acid obtained after acidification is carried out molecular distillation processing under conditions of 130~300 DEG C of temperature, 0.1~20Pa of vacuum degree, obtains white purification lanolin fatty acid.Added value of the present invention is high.Lanonol produced by the present invention, lanolin fatty acid are high-quality, and separative efficiency is high, to raw wool rouge wide adaptability, are suitble to industrialized production, application potential is huge.
Description
Technical field
The present invention relates to a kind of methods for preparing lanolin fatty acid and lanonol by lanolin, are especially prepared by lanolin high-purity
Spend the method for lanolin fatty acid and high quality lanonol.
Background technique
Lanolin mainly by the fatty acid of higher molecular weight (C7~C41) and approximately equal amounts of fatty alcohol (C12~C36),
In addition the unitary alcohol ester of the formation such as sterol, trimethyl sterol contains minimal amount of free acid, free alcohol, alkane and unknown material.Only
There is a small amount of lanolin crude product to be directly used in fields, most of high added values such as medicine, cosmetics and antirust agent after purification to spread out
Biology be saponified by lanolin after lanolin fatty acid and lanonol be made by the techniques such as separating, purifying, synthesize, such as lanolin fatty acid isopropyl
Pure and mild polyvinyl fluoride lanolin fatty acid of ester, acetylated lanolin etc., is widely used in medicine, cosmetics, chemical industry, weaving and leather
Etc. industries.It can be seen that the separation of lanolin fatty acid and lanonol seems most important, especially obtains high-purity after lanolin saponification
Spend lanolin fatty acid and high quality lanonol.
Currently, the method for extracting separation lanolin fatty acid and lanonol from lanolin mainly has solvent extraction, calcium soap conversion
Method, extraction-extraction coupled method.Wherein solvent extraction is most widely used, and the method is using lanolin fatty acid soap and lanonol in solvent
The difference of middle solubility and the separation for realizing lanolin fatty acid soap and lanonol, but it is low that emulsification, yield are easy in extraction process, and obtains
Lanonol it is second-rate.Lanolin fatty acid or lanolin fatty acid metallic soap are produced using lanolin, since lanolin itself contains pigment,
Under the high-temperature conditions such as saponification, acidification, pigment oxidation, color is deepened, while having certain peculiar smell, seriously affects the final of product
Quality.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
It the problem of in view of the above-mentioned and/or existing method for preparing lanolin fatty acid and lanonol by lanolin, proposes
The present invention.
Therefore, the one of purpose of the present invention is to overcome the existing method that lanolin fatty acid and lanonol are prepared by lanolin
Deficiency provides a kind of method for preparing lanolin fatty acid and lanonol by lanolin.
In order to solve the above technical problems, according to an aspect of the present invention, the present invention provides following technical solutions：It is a kind of
The method that lanolin fatty acid and lanonol are prepared by lanolin, it is characterised in that：Including,
Calcification：The saponification mixture obtained after lanolin is saponified, by salt acid for adjusting pH to 7~10, addition excessive 0~
50% calcium chloride solution carries out ion-exchange reactions under conditions of 40~80 DEG C of temperature, and reaction filters after 0.5~6 hour,
Wash cake layer into filtrate not chloride to get arrive lanolin fatty acid calcium and fatty alcohol mixture；
Alcohol is washed：The mixture of the lanolin fatty acid calcium and fatty alcohol that obtain after calcification is placed in reactor, addition quality is sheep
Hirsutic acid calcium and 2~20 times of fatty alcohol mixture of alcohol reagent, alcohol is washed under conditions of 55~80 DEG C, collects filtrate, recycles alcohol
Class solvent, obtains lanonol, and filter cake is lanolin fatty acid calcium；
Acidification：The lanolin fatty acid calcium obtained after alcohol is washed is placed in reactor, and organic reagent is added, then Plus acidic reagent is adjusted
PH is to acidity, branch vibration layer after reaction 1~6 hour, and organic layer is washed to neutrality, recycles organic solvent, obtains crude lanolin fatty acid；
Molecular distillation：The crude lanolin fatty acid obtained after acidification is subjected to molecular distillation processing, obtains light phase and heavy phase, light phase
As refine lanolin fatty acid.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Alcohol reagent is one or more of methanol, ethyl alcohol and isopropanol.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Alcohol is washed, alcohol wash the time be 1~4 hour, alcohol wash number be 1~5 time.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Organic reagent is one or more of n-hexane, petroleum ether, anhydrous ether and toluene.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Acid reagent is one or more of hydrochloric acid, sulfuric acid and phosphoric acid.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Acidification, temperature are 50~80 DEG C.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Molecular distillation, temperature are 130~300 DEG C, and vacuum degree is 0.1~20Pa.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：It is described
Molecular distillation, 175~230 DEG C of temperature, 0.1~5Pa of vacuum degree.
As a kind of preferred embodiment of the present invention for preparing lanolin fatty acid and lanonol method by lanolin, wherein：Also wrap
Include saponification, in reactor, lanolin and excessive 10~100% sodium hydroxide or potassium hydroxide in 2~6 times of volumes
Saponification is carried out in methanol, ethyl alcohol or isopropanol under conditions of 55~90 DEG C of temperature, reaction recycled alcohols after 4~16 hours
Solvent obtains saponification mixture.
Beneficial effects of the present invention：
1, excess base of the invention before calcification, after neutralization saponification in system, avoids calcification product lanolin fatty acid calcium
It is middle to introduce a large amount of calcium hydroxide, it is effectively reduced the amount of reagent that subsequent operation uses.
2, after the present invention is for lanolin saponification, alcohol soap is difficult to isolated status, increases alcohol after calcification and washes step, thoroughly has
The separation lanolin fatty acid calcium and lanonol of effect, obtain the lanonol of higher degree, can directly adopt the methods of crystallization, molecular distillation and mention
It takes steroidal compounds therein or directly prepares other lanolin derived products.
3, the present invention carries out sheep using molecular distillation technique for the drawback that lanolin fatty acid color is deep, peculiar smell is heavy is produced at present
The purification of hirsutic acid, the lanolin fatty acid isolated is with high purity, high-quality, and added value is high, can be directly used in the fields such as cosmetics.
4, separative efficiency of the present invention is high, and to raw wool rouge wide adaptability, inferior quality or the longer sheep of storage time
Hair rouge can be applicable in.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below with reference to specification embodiment
Specific embodiments of the present invention will be described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
100.0 grams of lanolin (saponification number 102.0) are slowly added into the sodium hydroxide (excess containing 8.7 grams
20%) it, in the reactor of 300 milliliters of ethyl alcohol, is stirred to react at 60 DEG C 4 hours, vacuum recycles ethyl alcohol.Saponification mixture is added
In 1 liter of reactor, using salt acid for adjusting pH to 8,11.1 grams of (excessive 10%) calcium chloride are dissolved in 100 ml deionized waters
In, it is added in reactor, is stirred to react at 40 DEG C 2 hours after dissolving completely, filtered, wash cake layer not chloride containing into filtrate
Object obtains 121.6 grams of mixture of lanolin fatty acid calcium and fatty alcohol.1 liter anti-is added in the mixture of lanolin fatty acid calcium and fatty alcohol
It answers in device, 729.6 milliliters of ethyl alcohol is added, are stirred 2 hours at 65 DEG C, alcohol is washed 3 times.Filtrate is collected, ethyl alcohol is recycled, obtains faint yellow
50.4 grams of lanonol, testing its acid value is 0.5, and saponification number 5.3, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 60 DEG C 2 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
48.4 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 200 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 0.2Pa, knifing rotating speed 120r/min, charging rate 1.2mL/min obtain white
40.2 grams of lanolin fatty acid of purification, testing its acid value is 168.4, and saponification number 172.3, product quality meets Europe and United States Pharmacopeia.
Embodiment 2
100.0 grams of degras (saponification number 90.4) are slowly added into the potassium hydroxide (excess containing 14.5 grams
100%) it, in the reactor of 400 ml methanols, is stirred to react at 65 DEG C 4 hours, vacuum recycles methanol.By saponification mixture plus
Enter in 1 liter of reactor, using salt acid for adjusting pH to 8,12.1 grams of (excessive 20%) calcium chloride are dissolved in 100 milliliters of deionizations
It in water, is added in reactor, is stirred to react at 50 DEG C 2 hours after dissolving completely, filtered, wash cake layer and be free of chlorine into filtrate
Compound obtains 114.8 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 1 liter
In reactor, 249.6 ml methanols are added, are stirred 3 hours at 60 DEG C, alcohol is washed 3 times.Filtrate is collected, methanol is recycled, obtains yellowish
43.4 grams of color lanonol, testing its acid value is 0.4, and saponification number 5.0, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of petroleum ethers are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 65 DEG C 2 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
46.4 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 210 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 0.1Pa, knifing rotating speed 130r/min, charging rate 1.0mL/min obtain white
43.2 grams of lanolin fatty acid of purification, testing its acid value is 165.4, and saponification number 170.2, product quality meets Europe and United States Pharmacopeia.
Embodiment 3
100.0 grams of lanolin (saponification number 102.0) are slowly added into the sodium hydroxide (excess containing 9.4 grams
30%) it, in the reactor of 400 milliliters of ethyl alcohol, is stirred to react at 70 DEG C 6 hours, vacuum recycles ethyl alcohol.Saponification mixture is added
In 1 liter of reactor, using salt acid for adjusting pH to 8,13.1 grams of (excessive 30%) calcium chloride are dissolved in 100 ml deionized waters
In, it is added in reactor, is stirred to react at 50 DEG C 3 hours after dissolving completely, filtered, wash cake layer not chloride containing into filtrate
Object obtains 131.2 grams of mixture of lanolin fatty acid calcium and fatty alcohol.1 liter anti-is added in the mixture of lanolin fatty acid calcium and fatty alcohol
It answers in device, 656 milliliters of ethyl alcohol is added, are stirred 2 hours at 65 DEG C, alcohol is washed 3 times.Filtrate is collected, ethyl alcohol is recycled, obtains faint yellow sheep
53.6 grams of alcohol of hair, testing its acid value is 0.4, and saponification number 5.0, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using sulphur acid for adjusting pH to acidity, is stirred to react at 70 DEG C 2 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
47.5 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 200 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, vacuum degree 2.6Pa, knifing rotating speed 90r/min, charging rate 1.8mL/min, obtains white essence
38.4 grams of lanolin fatty acid processed, testing its acid value is 163.3, and saponification number 170.5, product quality meets Europe and United States Pharmacopeia.
Embodiment 4
100.0 grams of lanolin (saponification number 102.0) are slowly added into the potassium hydroxide (excess containing 9.4 grams
30%) it, in the reactor of 400 milliliters of ethyl alcohol, is stirred to react at 90 DEG C 12 hours, vacuum recycles ethyl alcohol.By saponification mixture plus
Enter in 1 liter of reactor, using salt acid for adjusting pH to 8,14.1 grams of (excessive 40%) calcium chloride are dissolved in 100 milliliters of deionizations
It in water, is added in reactor, is stirred to react at 60 DEG C 4 hours after dissolving completely, filtered, wash cake layer and be free of chlorine into filtrate
Compound obtains 138.2 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 1 liter
In reactor, 552.8 milliliters of ethyl alcohol are added, are stirred 2 hours at 65 DEG C, alcohol is washed 5 times.Filtrate is collected, ethyl alcohol is recycled, obtains yellowish
57.6 grams of color lanonol, testing its acid value is 0.3, and saponification number 4.8, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of anhydrous second are added
Ether is stirred to react 4 hours using salt acid for adjusting pH to acidity at 60 DEG C, and organic layer is taken to be washed to neutrality, recycles organic solvent,
Obtain 50.5 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 160 DEG C of temperature, built-in condenser 20
DEG C, cold-trap is cooling using liquid nitrogen, and vacuum degree 4.6Pa, knifing rotating speed 90r/min, charging rate 2.0mL/min are obtained
34.8 grams of lanolin fatty acid of white purification, testing its acid value is 168.4, and saponification number 174.2, product quality meets Europe and U.S.'s medicine
Allusion quotation.
Embodiment 5
100.0 grams of lanolin (saponification number 102.0) are slowly added into containing 14.5 grams of sodium hydroxide is (excessive
100%) it, in the reactor of 600 milliliters of isopropanols, is stirred to react at 80 DEG C 10 hours, vacuum recycles isopropanol.Saponification is mixed
Object is added in 1 liter of reactor, using salt acid for adjusting pH to 9,14.1 grams of (excessive 40%) calcium chloride is dissolved in 100 milliliters and is gone
In ionized water, dissolve completely after be added reactor in, be stirred to react at 75 DEG C 4 hours, filter, wash cake layer into filtrate not
Chloride obtains 136.8 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 1
In the reactor risen, 273.6 ml methanols are added, are stirred 1 hour at 70 DEG C, alcohol is washed 2 times.Filtrate is collected, methanol is recycled, obtains
40.6 grams of faint yellow lanonol, testing its acid value is 0.5, and saponification number 5.4, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of toluene are added, make
It with salt acid for adjusting pH to acidity, is stirred to react 6 hours at 70 DEG C, organic layer is taken to be washed to neutrality, recycle organic solvent, obtained thick
55.8 grams of lanolin fatty acid processed.Crude lanolin fatty acid is refined by molecular distillation, 220 DEG C of temperature, 20 DEG C of built-in condenser, cold-trap
Cooling, vacuum degree 0.3Pa, knifing rotating speed 140r/min, charging rate 1.2mL/min using liquid nitrogen obtain white essence
53.6 grams of lanolin fatty acid processed, testing its acid value is 149.8, and saponification number 156.5, product quality meets Europe and United States Pharmacopeia.
Embodiment 6
100.0 grams of lanolin (saponification number 102.0) are slowly added into containing 10.8 grams of sodium hydroxide is (excessive
50%) it, in the reactor of 500 milliliters of ethyl alcohol, is stirred to react at 60 DEG C 8 hours, vacuum recycles ethyl alcohol.Saponification mixture is added
In 1 liter of reactor, using salt acid for adjusting pH to 7,12.1 grams of (excessive 20%) calcium chloride are dissolved in 100 ml deionized waters
In, it is added in reactor, is stirred to react at 45 DEG C 6 hours after dissolving completely, filtered, wash cake layer not chloride containing into filtrate
Object obtains 135.6 grams of mixture of lanolin fatty acid calcium and fatty alcohol.1 liter anti-is added in the mixture of lanolin fatty acid calcium and fatty alcohol
It answers in device, 406.8 milliliters of ethyl alcohol is added, are stirred 3 hours at 70 DEG C, alcohol is washed 5 times.Filtrate is collected, ethyl alcohol is recycled, obtains faint yellow
50.5 grams of lanonol, testing its acid value is 0.4, and saponification number 5.6, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 70 DEG C 2 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
50.6 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 230 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 2.4Pa, knifing rotating speed 130r/min, charging rate 1.5mL/min obtain white
45.2 grams of lanolin fatty acid of purification, testing its acid value is 160.4, and saponification number 166.7, product quality meets Europe and United States Pharmacopeia.
Embodiment 7
100.0 grams of lanolin (saponification number 102.0) are slowly added into containing 10.8 grams of sodium hydroxide is (excessive
50%) it, in the reactor of 500 milliliters of ethyl alcohol, is stirred to react at 80 DEG C 6 hours, vacuum recycles ethyl alcohol.Saponification mixture is added
In 1 liter of reactor, using salt acid for adjusting pH to 10,12.1 grams of (excessive 20%) calcium chloride are dissolved in 100 milliliters of deionizations
It in water, is added in reactor, is stirred to react at 45 DEG C 6 hours after dissolving completely, filtered, wash cake layer and be free of chlorine into filtrate
Compound obtains 130.6 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 5 liters
In reactor, 2612 milliliters of ethyl alcohol are added, are stirred 3 hours at 70 DEG C, alcohol is washed 3 times.Filtrate is collected, ethyl alcohol is recycled, obtains yellowish
51.4 grams of color lanonol, testing its acid value is 0.4, and saponification number 5.6, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 90 DEG C 2 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
49.6 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 130 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 2.4Pa, knifing rotating speed 120r/min, charging rate 1.5mL/min obtain white
21.2 grams of lanolin fatty acid of purification, testing its acid value is 168.4, and saponification number 177.4, product quality meets Europe and United States Pharmacopeia.
Embodiment 8
The lanolin (saponification number 106.4) that 100.0 grams store half a year is slowly added into containing by 13.0 grams of hydrogen-oxygen
In the reactor for changing sodium (excessive 80%), 500 milliliters of ethyl alcohol, it is stirred to react at 65 DEG C 10 hours, vacuum recycles ethyl alcohol.It will saponification
Mixture is added in 1 liter of reactor, and using salt acid for adjusting pH to 9,13.1 grams of (excessive 30%) calcium chloride are dissolved in 100 millis
It rises in deionized water, is added in reactor, is stirred to react at 65 DEG C 3 hours after dissolving completely, filtered, washing cake layer to filtrate
In not chloride, obtain 137.6 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added
Enter in 2 liters of reactor, 1376 milliliters of ethyl alcohol are added, are stirred 3 hours at 85 DEG C, alcohol is washed 4 times.Filtrate is collected, ethyl alcohol is recycled, obtains
To 53.9 grams of faint yellow lanonol, testing its acid value is 0.5, and saponification number 6.4, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium.Lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of toluene are added, make
It with salt acid for adjusting pH to acidity, is stirred to react 4 hours at 70 DEG C, organic layer is taken to be washed to neutrality, recycle organic solvent, obtained thick
49.8 grams of lanolin fatty acid processed.Crude lanolin fatty acid is refined by molecular distillation, 300 DEG C of temperature, 20 DEG C of built-in condenser, cold-trap
Cooling using liquid nitrogen, vacuum degree 20Pa, knifing rotating speed 110r/min, charging rate 1.0mL/min obtain white purification
44.6 grams of lanolin fatty acid, testing its acid value is 162.4, and saponification number 170.5, product quality meets Europe and United States Pharmacopeia.
Embodiment 9
100.0 grams of lanolin (saponification number 102.0) are slowly added into containing 13.0 grams of sodium hydroxide is (excessive
50%) it, in the reactor of 400 ml methanols, is stirred to react at 65 DEG C 16 hours, vacuum recycles methanol.By saponification mixture plus
Enter in 1 liter of reactor, using salt acid for adjusting pH to 7,12.1 grams of (excessive 20%) calcium chloride are dissolved in 100 milliliters of deionizations
It in water, is added in reactor, is stirred to react at 80 DEG C 1.5 hours after dissolving completely, filtered, washing cake layer is free of into filtrate
Chloride obtains 137.6 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 2 liters
Reactor in, 1100.8 milliliters of ethyl alcohol are added, are stirred 2 hours at 75 DEG C, alcohol is washed 3 times.Filtrate is collected, ethyl alcohol is recycled, obtains
50.9 grams of faint yellow lanonol, testing its acid value is 0.7, and saponification number 6.7, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 75 DEG C 3 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
50.6 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 200 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 10.5Pa, knifing rotating speed 150r/min, charging rate 1.2mL/min obtain white
45.0 grams of lanolin fatty acid of purification, testing its acid value is 169.8, and saponification number 178.9, product quality meets Europe and United States Pharmacopeia.
Embodiment 10
100.0 grams of lanolin (saponification number 102.0) are slowly added into containing 13.0 grams of sodium hydroxide is (excessive
50%) it, in the reactor of 400 milliliters of ethyl alcohol, is stirred to react at 65 DEG C 10 hours, vacuum recycles ethyl alcohol.By saponification mixture plus
Enter in 1 liter of reactor, using salt acid for adjusting pH to 8,12.1 grams of (excessive 20%) calcium chloride are dissolved in 100 milliliters of deionizations
It in water, is added in reactor, is stirred to react at 65 DEG C 3 hours after dissolving completely, filtered, wash cake layer and be free of chlorine into filtrate
Compound obtains 133.7 grams of mixture of lanolin fatty acid calcium and fatty alcohol.The mixture of lanolin fatty acid calcium and fatty alcohol is added 2 liters
In reactor, 1337 milliliters of ethyl alcohol are added, are stirred 3 hours at 70 DEG C, alcohol is washed 5 times.Filtrate is collected, ethyl alcohol is recycled, obtains yellowish
52.2 grams of color lanonol, testing its acid value is 0.4, and saponification number 6.2, product quality meets Europe and United States Pharmacopeia.
Filter cake is lanolin fatty acid calcium, and lanolin fatty acid calcium powder is added in 1 liter of reactor after broken, 200 milliliters of n-hexanes are added,
It using salt acid for adjusting pH to acidity, is stirred to react at 70 DEG C 4 hours, organic layer is taken to be washed to neutrality, recycled organic solvent, obtain
50.6 grams of crude lanolin fatty acid.Crude lanolin fatty acid is refined by molecular distillation, 150 DEG C of temperature, 20 DEG C of built-in condenser is cold
Trap is cooling using liquid nitrogen, and vacuum degree 2.4Pa, knifing rotating speed 130r/min, charging rate 1.5mL/min obtain white
29.1 grams of lanolin fatty acid of purification, testing its acid value is 165.4, and saponification number 174.7, product quality meets Europe and United States Pharmacopeia.
Since there are excessive alkali in system after lanolin is saponified, in subsequent calcification process, more hydrogen can be produced
Calcium oxide causes to increase the amount of reagent that subsequent operation uses containing more calcium hydroxide in lanolin fatty acid calcium.Add acid for adjusting pH
It is too low, cause lanolin fatty acid soap to be combined with acid and generate lanolin fatty acid, causes the reduction of lanolin fatty acid yield, it is therefore desirable to acid for adjusting pH be added
With a reasonable section.The same of lanolin fatty acid yield is being effectively ensured by hydrochloric acid regulation system pH to 7~10 in the present invention
When, reduce the amount of reagent that subsequent operation uses.
The saponification mixture that the present invention obtains after being saponified lanolin carries out calcification processing, and lanolin fatty acid soap is converted into lanolin fatty acid
Calcium precipitate.Since the fusing point of lanonol is 55 DEG C or so, the too low lanonol of temperature is solid-state, is wrapped in around lanolin fatty acid calcium,
It is not easy to wash away, temperature is excessively high, and alcohol is easy to cause to boil, and increases Operating Complexity.Therefore, the present invention explores after calcification processing
Optimal alcohol washes 55~80 DEG C of temperature out, washes at this temperature through carrying out alcohol, can effectively remove its surface lanonol.
Since lanolin itself contains pigment, during the processing such as saponification, acidification, under high-temperature condition, pigment is oxidizable,
Color is deepened, while having certain peculiar smell, seriously affects the final quality of product.Using conventional decoloration such as physisorphtion (silicon
Diatomaceous earth, active carbon etc.) meeting absorbing fats acid, the loss of lanolin fatty acid is caused, chemical decolorization method (hydrogen peroxide) introduces chemical reagent,
Later period is not easy to remove, and the lanolin fatty acid obtained after acidification progress molecular distillation is removed depigmentation by the present invention, preferred by experimental exploring
Molecular distillation parameter out obtains white lanolin fatty acid, does not introduce chemical reagent, and lanolin fatty acid loss is low, and gained lanolin fatty acid good quality,
Product quality reaches Europe and USP requirement.
In conclusion increase alcohol after the present invention is using lanolin saponification by hydrochloric acid system pH, and after calcification and wash step,
Lanolin fatty acid calcium and lanonol thoroughly are efficiently separated, obtains the lanonol of higher degree.It is carried out simultaneously using molecular distillation technique
The purification of lanolin fatty acid avoids the drawback for producing that lanolin fatty acid color is deep, peculiar smell is heavy in the past, lanolin fatty acid purity is high, the matter isolated
Amount is high, added value is high.Separative efficiency of the present invention is high, and to raw wool rouge wide adaptability, is suitble to industrialized production, application potential
It is huge.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (9)
1. a kind of method for preparing lanolin fatty acid and lanonol by lanolin, it is characterised in that：Including,
Calcification：The saponification mixture obtained after lanolin is saponified is added excessive 0~50% by salt acid for adjusting pH to 7~10
Calcium chloride solution carry out ion-exchange reactions under conditions of 40~80 DEG C of temperature, reaction filters after 0.5~6 hour, washes
Cake layer into filtrate not chloride to get arrive lanolin fatty acid calcium and fatty alcohol mixture；
Alcohol is washed：The mixture of the lanolin fatty acid calcium and fatty alcohol that obtain after calcification is placed in reactor, addition quality is lanolin fatty acid
Calcium and 2~20 times of fatty alcohol mixture of alcohol reagent, alcohol is washed under conditions of 55~80 DEG C, collects filtrate, and recycling alcohols is molten
Agent, obtains lanonol, and filter cake is lanolin fatty acid calcium；
Acidification：The lanolin fatty acid calcium obtained after alcohol is washed is placed in reactor, be added organic reagent, then Plus acidic reagent adjust pH to
Acidity, branch vibration layer after reaction 1~6 hour, organic layer are washed to neutrality, recycle organic solvent, obtain crude lanolin fatty acid；
Molecular distillation：The crude lanolin fatty acid obtained after acidification is subjected to molecular distillation processing, obtains light phase and heavy phase, light phase is
Refine lanolin fatty acid.
2. the method for preparing lanolin fatty acid and lanonol by lanolin as described in claim 1, it is characterised in that：The alcohols examination
Agent is one or more of methanol, ethyl alcohol and isopropanol.
3. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：The alcohol
Wash, alcohol wash the time be 1~4 hour, alcohol wash number be 1~5 time.
4. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：It is described to have
Machine reagent is one or more of n-hexane, petroleum ether, anhydrous ether and toluene.
5. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：The acid
Property reagent be one or more of hydrochloric acid, sulfuric acid and phosphoric acid.
6. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：The acid
Change, temperature is 50~80 DEG C.
7. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：Described point
Son distillation, temperature are 130~300 DEG C, and vacuum degree is 0.1~20Pa.
8. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：Described point
Son distillation, 175~230 DEG C of temperature, 0.1~5Pa of vacuum degree.
9. the method for preparing lanolin fatty acid and lanonol by lanolin as claimed in claim 1 or 2, it is characterised in that：Further include
Saponification, in reactor, lanolin and excessive 10~100% sodium hydroxide or potassium hydroxide 2~6 times of volumes first
Saponification is carried out in alcohol, ethyl alcohol or isopropanol under conditions of 55~90 DEG C of temperature, recycling alcohols is molten after reaction 4~16 hours
Agent obtains saponification mixture.
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