CN110002983A - A kind of method for making alpha, beta-lonone reduce isomerization in distillation process - Google Patents
A kind of method for making alpha, beta-lonone reduce isomerization in distillation process Download PDFInfo
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- CN110002983A CN110002983A CN201910338664.1A CN201910338664A CN110002983A CN 110002983 A CN110002983 A CN 110002983A CN 201910338664 A CN201910338664 A CN 201910338664A CN 110002983 A CN110002983 A CN 110002983A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/86—Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention provides a kind of methods for making alpha, beta-lonone reduce isomerization in distillation process, it is characterized in that, it include: that metal oxide or metal carbonate salt powder are added in the alpha, beta-lonone crude product of rectifying, rectifying is carried out in rectifying column, make to be in boiling to rectifying object in distillation process, oxidizes metal object or metal carbonate salt powder does not sink to rectifier bottoms.The present invention can preferably reduce alpha, beta-lonone heating distillation process in isomery at the ratio for being difficult isolated α-ionone, product yield is improved up to the alpha, beta-lonone of 72.5% (being higher than based on 94% by qualified product purity), meets the requirement as the raw material for preparing vitamin A.
Description
Technical field
The invention belongs to chemical field, it is related to the organic matter of easy isomerization during heating, especially to purity requirement
Very high pharmaceutical intermediate, as alpha, beta-lonone reduces the technology of isomerization.
Background technique
The method of rectifying alpha, beta-lonone has following several at present:
1. general vacuum degree (10~15mmHg), vapo(u)rizing temperature height (300 DEG C or more), the result is that yield is low (generally below
60%), purity is low, and isomerization is serious in distillation process, and major isomer is at being difficult isolated α-ionone (boiling point and β-purple
Only poor 2 DEG C of rowland ketone), for up to 35%.
2. condition of high vacuum degree (1mmHg or less), vapo(u)rizing temperature is medium (250 DEG C or so), and yield is higher (generally below 70%),
Purity is general, and isomerization is more serious in distillation process, and major isomer is at being difficult isolated α-ionone (boiling point and β-purple sieve
Only poor 2 DEG C of blue ketone), for up to 20%, and also operating cost is high.
As the medicine intermediate for preparing vitamin A, the purity of alpha, beta-lonone must reach 94% or more, otherwise can only
It scraps or the spice material much lower as price, will cause very big loss.
Summary of the invention
The object of the present invention is to provide a kind of methods for making alpha, beta-lonone reduce isomerization in distillation process.
In order to achieve the above object, the present invention provides the sides for making alpha, beta-lonone reduce isomerization in a kind of distillation process
Method characterized by comprising metal oxide or strong basicity metal carbonate salt powder are added thick to the alpha, beta-lonone of rectifying
In product, rectifying is carried out in rectifying column, is made to be in boiling to rectifying object in distillation process, is oxidized metal object or strong basicity metal
Carbonate powder does not sink to rectifier bottoms.
Preferably, the metal oxide or strong basicity metal carbonate be magnesia, calcium oxide, natrium carbonicum calcinatum or
Anhydrous potassium carbonate.
Preferably, based on the thick alpha, beta-lonone weight percent to rectifying, the additional amount of the magnesium oxide powder is 3
~10%.
Preferably, based on the thick alpha, beta-lonone weight percent to rectifying, the additional amount of the lime powder is 3
~10%.
Preferably, based on the thick alpha, beta-lonone weight percent to rectifying, the addition of the natrium carbonicum calcinatum powder
Amount is 3.0~7.0%.
Preferably, based on the thick alpha, beta-lonone weight percent to rectifying, the addition of the Anhydrous potassium carbonate powder
Amount is 2.5~5.5%.
Preferably, before being added magnesium oxide powder in the alpha, beta-lonone crude product to rectifying, first by metal oxide
Or strong basicity metal carbonate salt powder drying.
Preferably, after being added magnesium oxide powder in the alpha, beta-lonone crude product to rectifying, will be added with vacuum pump
Metal oxide or the alpha, beta-lonone crude product to rectifying of strong basicity metal carbonate salt powder are pumped into rectifying column.
Preferably, the distillation process includes: and first vacuumizes, and heating makes to be in fluidized state to rectifying object, makes metal
Oxide or strong basicity metal carbonate salt powder do not sink to rectifier bottoms, are then gradually warmed up fractionation, sampling analysis, wait slip out
When alpha, beta-lonone content reaches 92% in object, increase electric heating amplitude, collection slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.
It is highly preferred that described is evacuated to air pressure lower than 5mmHg.
Compared with prior art, the beneficial effects of the present invention are:
A certain proportion of metal oxide or strong basicity metal carbonate is added in the present invention in the alpha, beta-lonone to rectifying
Salt powder constructs the environment for making that alpha, beta-lonone is made to reduce isomerization in distillation process as anti-α isomerization agent, can
The preferable alpha, beta-lonone isomery in heating distillation process that reduces improves product at the ratio for being difficult isolated α-ionone
Yield meets up to the alpha, beta-lonone of 72.5% (being higher than based on 94% by qualified product purity) as the raw material for preparing vitamin A
It is required that.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Used each raw material is commercial product in following embodiment.
Embodiment 1-1
A kind of method for making alpha, beta-lonone reduce isomerization in distillation process, specific steps are as follows:
By the chemical pure zirconia magnesium bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape magnesia dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The magnesia that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of magnesium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that magnesia does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value, liquid because stablizing at this time, and temperature does not change), all collects and slips
For object until essence is slipped tower top temperature and reduced suddenly, slipping out object is the alpha, beta-lonone that content meets or exceeds 94% out.By to rectifying
Thick alpha, beta-lonone weight percent meter, weight such as the following table 1 of the present embodiment magnesia be added.
Embodiment 1-2
A kind of method for making alpha, beta-lonone reduce isomerization in distillation process, the specific steps are.
By the chemical pure zirconia magnesium bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape magnesia dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The magnesia that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of magnesium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that magnesia does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value) all collects and slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.Based on the thick alpha, beta-lonone weight percent to rectifying,
Weight such as the following table 1 of the present embodiment magnesia be added.
Embodiment 1-3
A kind of method for making alpha, beta-lonone reduce isomerization in distillation process, the specific steps are.
By the chemical pure zirconia magnesium bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape magnesia dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The magnesia that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of magnesium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that magnesia does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value) all collects and slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.Based on the thick alpha, beta-lonone weight percent to rectifying,
Weight such as the following table 1 of the present embodiment magnesia be added.
Comparative example 1-1: a method of so that alpha, beta-lonone is reduced isomerization, anti-isomerization agent magnesia powder is not added
End such as the following table 1.
By not plus magnesia in the thick alpha, beta-lonone of rectifying with vacuum be pumped into rectifying column in, pumping high vacuum is (to air pressure
Lower than 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that magnesia does not sink to bottom.Then it is gradually warmed up point
It evaporates.
- 1 yield of table and (in terms of 94% alpha, beta-lonone) and purity
Embodiment 2-1,
A kind of method of rectifying alpha, beta-lonone, specific steps are as follows:
By the chemical carbonate-free lime bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape calcium oxide dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The calcium oxide that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of calcium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that calcium oxide does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value) all collects and slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.Based on the thick alpha, beta-lonone weight percent to rectifying,
Weight such as the following table 1 of the present embodiment calcium oxide be added.
Embodiment 2-2
A kind of method of rectifying alpha, beta-lonone, the specific steps are.
By the chemical carbonate-free lime bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape calcium oxide dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The calcium oxide that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of calcium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that calcium oxide does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value) all collects and slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.Based on the thick alpha, beta-lonone weight percent to rectifying,
Weight such as the following table 1 of the present embodiment calcium oxide be added.
Embodiment 2-3
A kind of method of rectifying alpha, beta-lonone, the specific steps are.
By the chemical carbonate-free lime bought wear into 100 mesh powder (as product be in it is powdered if do not have to regrind).By powder
Shape calcium oxide dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.The calcium oxide that will be dried
Powder is added in the alpha, beta-lonone crude product to rectifying in stirring.The β-to rectifying of calcium peroxide powder will be added with vacuum pump
Irisone crude product is pumped into rectifying column and carries out rectifying, distillation process are as follows: pumping high vacuum (is lower than 5mmHg to air pressure), slightly hot
Just make to be in fluidized state to rectifying object, guarantees that calcium oxide does not sink to rectifier bottoms.Then fractionation, heating rate are gradually warmed up
It is about 5 DEG C/min, slips out object, and slips after tower top reaches 70~80 DEG C in essence that (related with vacuum degree, vacuum degree is about at this time
5mmHg), every 20 minutes sampling analyses increase electric heating amplitude when slipping out that alpha, beta-lonone content reaches 92% in object energetically
(conduction oil inlet and transformer voltage are raised to maximum value) all collects and slips out object until essence is slipped tower top temperature and dropped suddenly
Low, slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.Based on the thick alpha, beta-lonone weight percent to rectifying,
Weight such as the following table 1 of the present embodiment calcium oxide be added.
Comparative example 2-1: a method of so that alpha, beta-lonone is reduced isomerization, anti-isomerization agent calcium oxide powder is not added
End such as the following table 1.
By not plus calcium oxide in the thick alpha, beta-lonone of rectifying with vacuum be pumped into rectifying column in, pumping high vacuum is (to air pressure
Lower than 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that calcium oxide does not sink to bottom.Then it is gradually warmed up point
It evaporates.
- 1 yield of table and (in terms of 94% alpha, beta-lonone) and purity
Embodiment 3-1,
A method of improving alpha, beta-lonone purity, specific steps are as follows:
By the pure natrium carbonicum calcinatum of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous sodium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Natrium carbonicum calcinatum powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Natrium carbonicum calcinatum will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that natrium carbonicum calcinatum does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment natrium carbonicum calcinatum be added.
Embodiment 3-2
A method of alpha, beta-lonone purity is improved, the specific steps are.
By the pure natrium carbonicum calcinatum of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous sodium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Natrium carbonicum calcinatum powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Natrium carbonicum calcinatum will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that natrium carbonicum calcinatum does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment natrium carbonicum calcinatum be added.
Embodiment 3-3
A method of alpha, beta-lonone purity is improved, the specific steps are.
By the pure natrium carbonicum calcinatum of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous sodium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Natrium carbonicum calcinatum powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Natrium carbonicum calcinatum will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that natrium carbonicum calcinatum does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment natrium carbonicum calcinatum be added.
Comparative example 3-1: a method of so that alpha, beta-lonone is reduced isomerization, anti-isomerization agent Carbon Dioxide is not added
Sodium powder end such as the following table 1.
By not plus natrium carbonicum calcinatum in the thick alpha, beta-lonone of rectifying with vacuum be pumped into rectifying column in, pumping high vacuum is (extremely
Air pressure is lower than 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that natrium carbonicum calcinatum does not sink to bottom.Then by
The temperature that edges up fractionation.
- 1 yield of table and (in terms of 94% alpha, beta-lonone) and purity
Embodiment 4-1,
A method of producing alpha, beta-lonone, specific steps are as follows:
By the pure Anhydrous potassium carbonate of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous potassium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Anhydrous potassium carbonate powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Anhydrous potassium carbonate will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that Anhydrous potassium carbonate does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment Anhydrous potassium carbonate be added.
Embodiment 4-2
A method of alpha, beta-lonone is produced, the specific steps are.
By the pure Anhydrous potassium carbonate of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous potassium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Anhydrous potassium carbonate powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Anhydrous potassium carbonate will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that Anhydrous potassium carbonate does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment Anhydrous potassium carbonate be added.
Embodiment 4-3
A method of alpha, beta-lonone is produced, the specific steps are.
By the pure Anhydrous potassium carbonate of chemistry bought wear into 100 mesh powder (as product be in it is powdered just without regrinding).It will
Powdered anhydrous potassium carbonate dries 3 hours for use for 120 DEG C in an oven, as stand-by in being put into drier if not in time.It will dry
Anhydrous potassium carbonate powder be added in stirring in the alpha, beta-lonone crude product to rectifying.Anhydrous potassium carbonate will be added with vacuum pump
The alpha, beta-lonone crude product to rectifying of powder, which is pumped into rectifying column, carries out rectifying, distillation process are as follows: pumping high vacuum is (low to air pressure
In 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that Anhydrous potassium carbonate does not sink to rectifier bottoms.Then by
The temperature that edges up fractionation, heating rate is about 5 DEG C/min, slips out object, and slip after tower top reaches 70~80 DEG C (with vacuum degree in essence
Related, vacuum degree is about 5mmHg at this time), every 20 minutes sampling analyses reach 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude (conduction oil inlet and transformer voltage are raised to maximum value) energetically, all it is straight to slip out object for collection
Slipping tower top temperature suddenly to essence reduces, and slipping out object is the alpha, beta-lonone that content meets or exceeds 94%.By the thick β-to rectifying
Irisone weight percent meter, weight such as the following table 1 of the present embodiment Anhydrous potassium carbonate be added.
Comparative example 4-1: a method of so that alpha, beta-lonone is reduced isomerization, anti-isomerization agent Carbon Dioxide is not added
Potassium powder such as the following table 1.
By not plus Anhydrous potassium carbonate in the thick alpha, beta-lonone of rectifying with vacuum be pumped into rectifying column in, pumping high vacuum is (extremely
Air pressure is lower than 5mmHg), it is slightly hot just to make to be in fluidized state to rectifying object, guarantee that Anhydrous potassium carbonate does not sink to bottom.Then by
The temperature that edges up fractionation.
- 1 yield of table and (in terms of 94% alpha, beta-lonone) and purity
Claims (10)
1. a kind of method for making alpha, beta-lonone reduce isomerization in distillation process characterized by comprising by metal oxide
Or metal carbonate salt powder is added to carry out rectifying in rectifying column, make in distillation process in the alpha, beta-lonone crude product of rectifying
It is in boiling to rectifying object, object is oxidized metal or metal carbonate salt powder does not sink to rectifier bottoms.
2. the method for making alpha, beta-lonone reduce isomerization in distillation process as described in claim 1, which is characterized in that described
Metal oxide or carbonate be magnesia, calcium oxide, natrium carbonicum calcinatum or Anhydrous potassium carbonate.
3. make in distillation process as claimed in claim 2 alpha, beta-lonone reduce isomerization method, which is characterized in that by
The thick alpha, beta-lonone weight percent meter of rectifying, the additional amount of the magnesium oxide powder are 3~10%.
4. make in distillation process as claimed in claim 2 alpha, beta-lonone reduce isomerization method, which is characterized in that by
The thick alpha, beta-lonone weight percent meter of rectifying, the additional amount of the lime powder are 3~10%.
5. make in distillation process as claimed in claim 2 alpha, beta-lonone reduce isomerization method, which is characterized in that by
The thick alpha, beta-lonone weight percent meter of rectifying, the additional amount of the natrium carbonicum calcinatum powder are 3.0~7.0%.
6. make in distillation process as claimed in claim 2 alpha, beta-lonone reduce isomerization method, which is characterized in that by
The thick alpha, beta-lonone weight percent meter of rectifying, the additional amount of the Anhydrous potassium carbonate powder are 2.5~5.5%.
7. the method for making alpha, beta-lonone reduce isomerization in distillation process as described in claim 1, which is characterized in that inciting somebody to action
Magnesium oxide powder is added to first dry metal oxide or metal carbonate salt powder before in the alpha, beta-lonone crude product of rectifying
It is dry.
8. the method for making alpha, beta-lonone reduce isomerization in distillation process as described in claim 1, which is characterized in that inciting somebody to action
Magnesium oxide powder is added to add metal oxide or metal carbonate with vacuum pump after in the alpha, beta-lonone crude product of rectifying
The alpha, beta-lonone crude product to rectifying of salt powder is pumped into rectifying column.
9. the method for making alpha, beta-lonone reduce isomerization in distillation process as described in claim 1, which is characterized in that described
Distillation process include: first to vacuumize, heating make to be in fluidized state to rectifying object, oxidize metal object or metal carbonate salt fines
Rectifier bottoms are not sunk at end, are then gradually warmed up fractionation, sampling analysis reaches 92% wait slip out alpha, beta-lonone content in object
When, increase electric heating amplitude, collection slips out object and reduces suddenly up to essence slips tower top temperature, slips out object and meet or exceed for content
94% alpha, beta-lonone.
10. the method for making alpha, beta-lonone reduce isomerization in distillation process as claimed in claim 9, which is characterized in that institute
That states is evacuated to air pressure lower than 5mmHg.
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Citations (2)
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| CN104892381A (en) * | 2015-04-29 | 2015-09-09 | 上虞新和成生物化工有限公司 | C14 aldehyde distillation low boiling byproduct recycling method |
| CN106831382A (en) * | 2016-12-26 | 2017-06-13 | 广州百花香料股份有限公司 | A kind of preparation method for improving αisomer yield in irisone product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892381A (en) * | 2015-04-29 | 2015-09-09 | 上虞新和成生物化工有限公司 | C14 aldehyde distillation low boiling byproduct recycling method |
| CN106831382A (en) * | 2016-12-26 | 2017-06-13 | 广州百花香料股份有限公司 | A kind of preparation method for improving αisomer yield in irisone product |
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| 束铭杰等: "NaHSO3法分离紫罗兰酮异构体过程研究", 《现代化工》 * |
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