CN106699831B - A method of liquid crystal cholesterol is prepared using lanolin using complexometry - Google Patents

A method of liquid crystal cholesterol is prepared using lanolin using complexometry Download PDF

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CN106699831B
CN106699831B CN201611222997.0A CN201611222997A CN106699831B CN 106699831 B CN106699831 B CN 106699831B CN 201611222997 A CN201611222997 A CN 201611222997A CN 106699831 B CN106699831 B CN 106699831B
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cholesterol
lanolin
filtering
liquid crystal
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CN106699831A (en
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马志军
薛家禄
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Big Biological Medicine Co Of Henan Profit Limited-Liability Co
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Big Biological Medicine Co Of Henan Profit Limited-Liability Co
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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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K19/00—Liquid crystal materials
    • C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
    • C09K19/36—Steroidal liquid crystal compounds

Abstract

The invention discloses a kind of methods for preparing liquid crystal cholesterol using lanolin using complexometry, comprising the following steps: saponification, thin film evaporation, molecular distillation, complexing, solution complexing, crystallization, pickling, alkali cleaning, neutrality are washed and dried.In saponification, the feed way of water phase will be added to using oil, can solve the problem of alkali reacted with lanolin periphery form film make inside lanolin can not come into full contact with and react with alkali, saponification rate reaches 90%；The present invention prepares liquid crystal cholesterol using lanolin using complexometry, and with cholesterol yield, high, content is up to 98.5%, lower production costs, is suitble to industrialized production liquid crystal.

Description

A method of liquid crystal cholesterol is prepared using lanolin using complexometry
Technical field
The invention belongs to field of biotechnology, prepare liquid crystal gallbladder using lanolin using complexometry more particularly to a kind of The method of sterol.
Background technique
Cholesterol also known as lipidol of gallbladder, cholesterine are a kind of natural steroidal resources, are the main raw material(s)s of liquid crystal industry. Lanolin is a kind of smegma of sheep comes out, grease for being attached on wool, about containing 10% or so in lanolin Cholesterol.Extract cholesteric method from lanolin at present and be roughly divided into five classes: chromatography, molecularly distilled, surpasses bromination method Critical extraction, solvent selection crystallisation and matching method, since lanolin is easy emulsifier, the wool obtained by each method Rouge cholesterol level is below 96%, and impurity content is larger.But liquid crystal cholesterol is very severe to the quality requirement of product It carves, generally requires content 98% or more, it is therefore desirable to provide a kind of new technique for preparing liquid crystal cholesterol using lanolin Route, to produce qualified liquid crystal cholesterol.
Summary of the invention
The object of the invention is that overcome above-mentioned deficiency, provide a kind of cholesterol yield is high, content is high, production cost compared with The method for preparing liquid crystal cholesterol using lanolin that is low, being suitble to industrialized production.
In order to achieve the above objectives, the present invention is implemented according to following technical scheme:
A method of liquid crystal cholesterol is prepared using lanolin using complexometry, comprising the following steps:
S1. it is saponified, suitable sodium hydroxide solution is added into saponification kettle, heating stirring is slowly added to the wool of fusing Rouge is persistently stirred at reflux 8h；
S2. thin film evaporation, thin film evaporator carry out thin film evaporation；
S3. molecular distillation carries out molecular distillation into molecular distillation system；
S4. it is complexed, into complexing kettle, suitable ethyl acetate is added, preheat, suitable methanol and chlorine is then added Change calcium, stirring carries out complex reaction, is cooled to 22-25 DEG C after the reaction was completed, complex compound sufficient crystallising is precipitated, the acetic acid of addition The weight ratio of ethyl ester and calcium chloride is 4:1-8:1, and the methanol of addition and the weight ratio of calcium chloride are 1:3-1:1；
S5. solution complexing, filters out complex compound, is washed with ethyl acetate；A certain amount of purified water is added and ethyl acetate stirs Mix dissolution complex compound, separate organic layer, with purifying water washing organic layer；True evaporative air organic solvent obtains thick cholesterol；
S6. it crystallizes, above-mentioned thick cholesterol is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, is heated to 78 DEG C, adds Enter 1.5% active carbon, flows back 1 hour.Heat filtering, filtrate are put into crystallizing tank.Crystallisation by cooling.Filtering, drying；
Gained cholesterol in step S6 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added, adjusts PH by S7. pickling Value is 2-4, is dissolved by heating, and flow back 1-2h, crystallisation by cooling, filtering；
Gained cholesterol in step S7 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added, adjusts PH by S8. alkali cleaning Value is 9-13, is dissolved by heating, and flow back 1-2h, crystallisation by cooling, filtering；
S9. neutrality is washed, and gained cholesterol in step S8 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added, adjusts PH value is 7-8, is dissolved by heating, and suitable active carbon is added, and flow back 1-2h, filtering, by filtrate crystallisation by cooling, filtering；
S10. it dries.
Further, thin film evaporation condition are as follows: vacuum degree 0.09-0.092MPa, temperature are 145-150 DEG C.
Further, molecular distillation condition are as follows: vacuum degree 1-50Pa, temperature are 145-150 DEG C.
Further, the condition of complex reaction are as follows: temperature is 40-60 DEG C, reaction time 0.5-1h.
Compared with prior art, the invention has the benefit that
1, in saponification, it will be added to the feed way of water phase using oil, alkali can be solved with lanolin periphery and react knot Film forming makes the lanolin of the inside that can not come into full contact with the problem of reacting with alkali, and saponification rate reaches 90%；
2, liquid crystal cholesterol is prepared using lanolin using complexometry, cholesterol yield is high, content is up to 98.5%, life Cost is relatively low for production, is suitble to industrialized production.
Figure of description
Fig. 1 is process flow chart of the invention.
Specific embodiment
The invention will be further described with specific embodiment with reference to the accompanying drawings of the specification, in the schematic reality of the invention It applies example and explanation is used to explain the present invention, but is not as a limitation of the invention.
Embodiment 1
According to the process flow chart of Fig. 1, it includes following for preparing liquid crystal cholesterol using lanolin using complexometry Step:
S1. it is saponified, suitable sodium hydroxide solution is added into saponification kettle, heating stirring is slowly added to the wool of fusing Rouge is persistently stirred at reflux 8h；
S2. thin film evaporation, thin film evaporator carry out thin film evaporation, thin film evaporation condition are as follows: vacuum degree 0.09MPa, temperature Degree is 145 DEG C；
S3. molecular distillation carries out molecular distillation, molecular distillation condition into molecular distillation system are as follows: vacuum degree is 50Pa, temperature are 145 DEG C；
S4. it is complexed, into complexing kettle, suitable ethyl acetate is added, preheat, suitable methanol and chlorine is then added Change calcium, stirring carries out complex reaction, is cooled to 22 DEG C after the reaction was completed, complex compound sufficient crystallising is precipitated, the acetic acid second of addition The weight ratio of ester and calcium chloride is 4:1, and the methanol of addition and the weight ratio of calcium chloride are 1:3, the condition of complex reaction are as follows: temperature It is 40 DEG C, reaction time 0.5h；
S5. solution complexing, filters out complex compound, is washed with ethyl acetate；A certain amount of purified water is added and ethyl acetate stirs Mix dissolution complex compound, separate organic layer, with purifying water washing organic layer；True evaporative air organic solvent obtains thick cholesterol；
S6. it crystallizes, above-mentioned thick cholesterol is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, is heated to 78 DEG C, adds Enter 1.5% active carbon, flows back 1 hour.Heat filtering, filtrate are put into crystallizing tank.Crystallisation by cooling.Filtering, drying；
Gained cholesterol in step S6 is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, adjusts pH value by S7. pickling It is 2, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
Gained cholesterol in step S7 is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, adjusts pH value by S8. alkali cleaning It is 9, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
S9. neutrality is washed, and gained cholesterol in step S8 is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, adjusts PH Value is 7, is dissolved by heating, and suitable active carbon is added, and flow back 2h, filtering, by filtrate crystallisation by cooling, filtering；
S10. it dries.
Embodiment 2
According to the process flow chart of Fig. 1, cholesterol using lanolin is prepared using complexometry the following steps are included:
S1. it is saponified, suitable sodium hydroxide solution is added into saponification kettle, heating stirring is slowly added to the wool of fusing Rouge is persistently stirred at reflux 8h；
S2. thin film evaporation, thin film evaporator carry out thin film evaporation, thin film evaporation condition are as follows: vacuum degree 0.09MPa, temperature Degree is 150 DEG C；
S3. molecular distillation carries out molecular distillation, molecular distillation condition into molecular distillation system are as follows: vacuum degree is 50Pa, temperature are 150 DEG C；
S4. it is complexed, into complexing kettle, suitable ethyl acetate is added, preheat, suitable methanol and chlorine is then added Change calcium, stirring carries out complex reaction, is cooled to 22 DEG C after the reaction was completed, complex compound sufficient crystallising is precipitated, the acetic acid second of addition The weight ratio of ester and calcium chloride is 8:1, and the methanol of addition and the weight ratio of calcium chloride are 1:3, the condition of complex reaction are as follows: temperature It is 40 DEG C, reaction time 1h；
S5. solution complexing, filters out complex compound, is washed with ethyl acetate；A certain amount of purified water is added and ethyl acetate stirs Mix dissolution complex compound, separate organic layer, with purifying water washing organic layer；True evaporative air organic solvent obtains thick cholesterol；
S6. it crystallizes, above-mentioned thick cholesterol is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, is heated to 78 DEG C, adds Enter 1.5% active carbon, flows back 1 hour.Heat filtering, filtrate are put into crystallizing tank.Crystallisation by cooling.Filtering, drying；
Gained cholesterol in step S6 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts pH value by S7. pickling It is 4, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
Gained cholesterol in step S7 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts pH value by S8. alkali cleaning It is 13, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
S9. neutrality is washed, and gained cholesterol in step S8 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts PH Value is 7, is dissolved by heating, and suitable active carbon is added, and flow back 2h, filtering, by filtrate crystallisation by cooling, filtering；
S10. it dries.
Embodiment 3
According to the process flow chart of Fig. 1, cholesterol using lanolin is prepared using complexometry the following steps are included:
S1. it is saponified, suitable sodium hydroxide solution is added into saponification kettle, heating stirring is slowly added to the wool of fusing Rouge is persistently stirred at reflux 8h；
S2. thin film evaporation, thin film evaporator carry out thin film evaporation, thin film evaporation condition are as follows: vacuum degree 0.09MPa, temperature Degree is 150 DEG C；
S3. molecular distillation carries out molecular distillation, molecular distillation condition into molecular distillation system are as follows: vacuum degree is 50Pa, temperature are 150 DEG C；
S4. it is complexed, into complexing kettle, suitable ethyl acetate is added, preheat, suitable methanol and chlorine is then added Change calcium, stirring carries out complex reaction, is cooled to 25 DEG C after the reaction was completed, complex compound sufficient crystallising is precipitated, the acetic acid second of addition The weight ratio of ester and calcium chloride is 4:1, and the methanol of addition and the weight ratio of calcium chloride are 1:1, the condition of complex reaction are as follows: temperature It is 60 DEG C, reaction time 1h；
S5. solution complexing, filters out complex compound, is washed with ethyl acetate；A certain amount of purified water is added and ethyl acetate stirs Mix dissolution complex compound, separate organic layer, with purifying water washing organic layer；True evaporative air organic solvent obtains thick cholesterol；
S6. it crystallizes, above-mentioned thick cholesterol is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, is heated to 78 DEG C, adds Enter 1.5% active carbon, flows back 1 hour.Heat filtering, filtrate are put into crystallizing tank.Crystallisation by cooling.Filtering, drying；
Gained cholesterol in step S6 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts pH value by S7. pickling It is 2, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
Gained cholesterol in step S7 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts pH value by S8. alkali cleaning It is 10, dissolves by heating, flows back 2h, crystallisation by cooling, filtering；
S9. neutrality is washed, and gained cholesterol in step S8 is added in reaction kettle, the ethyl alcohol of 10 times of weight is added, adjusts PH Value is 8, is dissolved by heating, and suitable active carbon is added, and flow back 2h, filtering, by filtrate crystallisation by cooling, filtering；
S10. it dries.
The limitation that technical solution of the present invention is not limited to the above specific embodiments, it is all to do according to the technique and scheme of the present invention Technology deformation out, falls within the scope of protection of the present invention.

Claims (4)

1. a kind of method for preparing liquid crystal cholesterol using lanolin using complexometry, which comprises the following steps:
S1. it being saponified, suitable sodium hydroxide solution is added into saponification kettle, heating stirring is slowly added to the lanolin of fusing, Persistently it is stirred at reflux 8h；
S2. thin film evaporation, thin film evaporator carry out thin film evaporation；
S3. molecular distillation carries out molecular distillation into molecular distillation system；
S4. it is complexed, into complexing kettle, suitable ethyl acetate is added, preheat, suitable methanol and calcium chloride is then added, Stirring carries out complex reaction, is cooled to 22-25 DEG C after the reaction was completed, complex compound sufficient crystallising is precipitated, the ethyl acetate of addition Weight ratio with calcium chloride is 4:1-8:1, and the methanol of addition and the weight ratio of calcium chloride are 1:3-1:1；
S5. solution complexing, filters out complex compound, is washed with ethyl acetate；A certain amount of purified water is added and ethyl acetate stirring is molten Solve complex compound, separate organic layer, with purifying water washing organic layer；True evaporative air organic solvent obtains thick cholesterol；
S6. it crystallizes, above-mentioned thick cholesterol is added in reaction kettle, the ethyl alcohol of 20 times of weight is added, is heated to 78 DEG C, is added 1.5% active carbon flows back 1 hour；Heat filtering, filtrate are put into crystallizing tank；Crystallisation by cooling；Filtering, drying；
Gained cholesterol in step S6 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added by S7. pickling, and adjusting pH value is 2-4 is dissolved by heating, and flow back 1-2h, crystallisation by cooling, filtering；
Gained cholesterol in step S7 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added by S8. alkali cleaning, and adjusting pH value is 9-13 is dissolved by heating, and flow back 1-2h, crystallisation by cooling, filtering；
S9. neutrality is washed, and gained cholesterol in step S8 is added in reaction kettle, the ethyl alcohol of 8-20 times of weight is added, adjusts pH value It for 7-8, dissolves by heating, suitable active carbon is added, flow back 1-2h, filtering, by filtrate crystallisation by cooling, filtering；
S10. it dries.
2. the method for preparing liquid crystal cholesterol using lanolin using complexometry according to claim 1, which is characterized in that Thin film evaporation condition are as follows: vacuum degree 0.09-0.092MPa, temperature are 145-150 DEG C.
3. the method for preparing liquid crystal cholesterol using lanolin using complexometry according to claim 1, which is characterized in that Molecular distillation condition are as follows: vacuum degree 1-50Pa, temperature are 145-150 DEG C.
4. the method for preparing liquid crystal cholesterol using lanolin using complexometry according to claim 1, which is characterized in that The condition of complex reaction are as follows: temperature is 40-60 DEG C, reaction time 0.5-1h.
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Publication number Priority date Publication date Assignee Title
CN108864240B (en) * 2018-05-29 2020-03-24 湖南新合新生物医药有限公司 Method for purifying dexamethasone epoxy hydrolysate
CN111171098B (en) * 2020-01-14 2021-05-07 江西天新药业股份有限公司 Method for preparing cholesterol by using lanolin
CN113735931A (en) * 2021-08-27 2021-12-03 浙江花园营养科技有限公司 Method for separating cholesterol and 24-dehydrocholesterol by complexing crystallization

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1594350A (en) * 2004-06-24 2005-03-16 浙江大学 Method for separating and extracting cholesterol from lanolin
CN102690312A (en) * 2012-05-24 2012-09-26 河南利伟生物药业股份有限公司 Purification method for lanolin cholesterol
CN102863315A (en) * 2012-09-29 2013-01-09 杭州下沙生物科技有限公司 Method of using lanolin to prepare wool acid metal soap and lanonol
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
CN103554207A (en) * 2013-10-30 2014-02-05 吉安荣威生物科技有限公司 Lanolin cholesterol production technology

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1594350A (en) * 2004-06-24 2005-03-16 浙江大学 Method for separating and extracting cholesterol from lanolin
CN102690312A (en) * 2012-05-24 2012-09-26 河南利伟生物药业股份有限公司 Purification method for lanolin cholesterol
CN102863315A (en) * 2012-09-29 2013-01-09 杭州下沙生物科技有限公司 Method of using lanolin to prepare wool acid metal soap and lanonol
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
CN103554207A (en) * 2013-10-30 2014-02-05 吉安荣威生物科技有限公司 Lanolin cholesterol production technology

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