CN107459455A - A kind of method that methyl stearate is extracted in the benzoyl methane raffinate from stearic acid - Google Patents
A kind of method that methyl stearate is extracted in the benzoyl methane raffinate from stearic acid Download PDFInfo
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- CN107459455A CN107459455A CN201610383201.3A CN201610383201A CN107459455A CN 107459455 A CN107459455 A CN 107459455A CN 201610383201 A CN201610383201 A CN 201610383201A CN 107459455 A CN107459455 A CN 107459455A
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- methyl stearate
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a kind of method that methyl stearate is extracted in benzoyl methane raffinate from stearic acid, belong to field of chemical engineering.SBM raffinates is are introduced into vacuum rectification tower by concrete scheme, and after rectification under vacuum, tower top flows out the component than methyl stearate low boiling point, and methyl stearate and heavy constituent are flowed out by bottom of towe.Bottom stream by liquid-liquid extraction, isolates purity up to more than 85% methyl stearate again.The methyl stearate of this method isolated purity more than 85% from stearic acid benzoyl raffinate, while yield can reach more than 85%.Compared with the prior art, this method technique is simple, easy to operate, obtains methyl stearate purity and yield is higher.
Description
Technical field
The invention belongs to field of chemical engineering, and in particular to one kind is extracted from stearic acid benzoyl methane raffinate
The method of methyl stearate.
Background technology
The production method of stearoyl benzoyl methane (SBM), it is by acetophenone, methyl stearate and methanol
Obtained solid crude product is dissolved in recrystallisation solvent and tied by being condensed, be acidified, after concentration step by sodium
Crystalline substance, stearoyl benzoyl methane product is obtained after the crystallized product drying that will filter out.Stearoyl benzoyl first
Alkane (SBM) raffinate is in SBM production processes, and after Crystallization Separation product, mother liquor is through being distilled to recover solvent
Remaining raffinate, the content about 60% of methyl stearate in raffinate, but SBM raffinate complicated components, greatly
Multi-component boiling point is higher, it is difficult to isolate methyl stearate therein.Patent CN201210332441 is disclosed
A kind of method that methyl stearate is extracted in the raffinate from SBM, using the method for methanol extraction crystallization from SBM
In raffinate, but the content of methyl stearate that its extraction obtains is relatively low, because its process is more complicated, stearic acid
The yield of methyl esters is relatively low.
The content of the invention
The present invention is directed to extracts the purity of methyl stearate and the present situation that yield is relatively low from SBM raffinates at present,
A kind of method for being evaporated under reduced pressure and being combined with extraction phase is proposed, methyl stearate is separated from SBM raffinates.
SBM raffinates composition is complicated, and boiling point is close, at relatively high temperatures can coking, emphasis of the present invention is stearic in separation
During sour methyl esters, relatively low temperature is kept, therefore using in the method enrichment SBM raffinates of rectification under vacuum
Methyl stearate, it is follow-up that the higher methyl stearate of purity is obtained using extraction process.This method technique is simple,
It is easy to operate, the methyl stearate that purity is more than 85% can be proposed from SBM raffinates, while yield is reachable
To more than 85%.
Technical scheme proposed by the present invention is：
(1) it is evaporated under reduced pressure：Stearoyl benzoyl methane raffinate is introduced into vacuum rectification tower, vacuum rectification tower
Pressure 0.6KPa~10KPa, bottom temperature are 160 DEG C~200 DEG C, and vacuum rectification tower number of theoretical plate is 20 pieces
- 40 pieces, reflux ratio is 2~5, and after rectification under vacuum, tower top flows out the component than methyl stearate low boiling point,
Methyl stearate and heavy constituent are flowed out by bottom of towe；
(2) liquid-liquid extraction：Methyl stearate pregnant solution is introduced into extraction tower, extraction tower operation temperature is
20 DEG C~60 DEG C, extractant is 1~3: 1 with methyl stearate pregnant solution mass ratio, methyl stearate pregnant solution
Entering from tower top, extractant enters from tower bottom, after counter-current extraction, bottom of towe outflow methyl stearate.
In above-mentioned technical proposal, rectification under vacuum pressure tower 0.6KPa~10KPa, vacuum rectification tower number of theoretical plate
For 20~40 pieces, reflux ratio is 2~5, and bottom temperature is 160 DEG C~200 DEG C.
In above-mentioned technical proposal, described extractant is the organic solvent such as sulfolane, 1-METHYLPYRROLIDONE.
Extraction tower operation temperature be 20 DEG C~60 DEG C, extraction tower number of theoretical plate be 8~12 pieces, extractant with it is to be extracted
Solution quality ratio is 1~3: 1.
SBM raffinates are introduced into vacuum rectification tower, after rectification under vacuum, tower top outflow is boiled than methyl stearate
The low component of point, methyl stearate and heavy constituent are flowed out by bottom of towe.Bottom stream again by liquid-liquid extraction,
Purity is isolated up to more than 85% methyl stearate.
Specifically, it is as follows to be evaporated under reduced pressure the step of separating SBM raffinates with the method that liquid-liquid extraction is combined：
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is more than 20 pieces, keeps essence
It is 0.6KPa~10KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C~200 DEG C, and reflux ratio is 2~5, is passed through
It is evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, tower reactor outflow methyl stearate pregnant solution.Will be hard
Resin acid methyl ester rich liquid is introduced into extraction tower, and extraction tower operation temperature is 20 DEG C~60 DEG C, extraction tower theoretical plate
Number is 8~12 pieces, and extractant is 1~3: 1 with methyl stearate pregnant solution mass ratio, methyl stearate enrichment
Liquid enters from tower top, and extractant enters from tower bottom, and after counter-current extraction, bottom of towe outflow purity is 85%
Methyl stearate.
Beneficial effect
SBM raffinates composition is complicated, and boiling point is close, and most of component boiling point is higher, can tie at relatively high temperatures
Jiao, using rectification under vacuum carry out methyl stearate enrichment on the one hand can improve it is relatively volatile between separate substance
Degree, is advantageous to the enrichment of methyl stearate, while during rectification under vacuum, tower reactor operation temperature is relatively low,
The coking of high boiling substance can be prevented.The method that methyl stearate pregnant solution is extracted by normal temperature, height can be reduced
Boilers coking.Compared with prior art, the advantage of the invention is that using vacuum distillation and liquid-liquid extraction
The technique being combined, technique is simple, easy to operate, can be obtained from stearoyl benzoyl methane raffinate purity compared with
High methyl stearate.
Embodiment
The embodiment of the present invention is described in detail below, it should be noted however that this hair
Bright protection domain is not limited to these specific embodiments, but is determined by claims.
Embodiment 1
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 88%, stearic acid
The yield of methyl esters is 90%.
Embodiment 2
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 10KPa to evaporate tower tower pressure, and bottom temperature is 200 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 88%, stearic acid
The yield of methyl esters is 90%.
Embodiment 3
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 40 pieces, keeps essence
It is 10KPa to evaporate tower tower pressure, and bottom temperature is 200 DEG C, reflux ratio 3, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 88%, stearic acid
The yield of methyl esters is 90%.
Embodiment 4
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 2, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 73%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 85%, stearic acid
The yield of methyl esters is 92%.
Embodiment 5
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 1: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 85%, stearic acid
The yield of methyl esters is 90%.
Embodiment 6
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, N- methyl
Pyrrolidones enters from tower bottom, and 1-METHYLPYRROLIDONE is 3: 1 with methyl stearate mass ratio, extraction tower
Number of theoretical plate is 10 pieces, and extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe outflow purity is 87%
Methyl stearate, the yield of methyl stearate is 90%.
Embodiment 7
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 20 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 85%, stearic acid
The yield of methyl esters is 90%.
Embodiment 8
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, sulfolane
Entering from tower bottom, sulfolane is 3: 1 with methyl stearate mass ratio, and extraction tower number of theoretical plate is 10 pieces,
Extraction temperature is 60 DEG C, and after counter-current extraction, bottom of towe flows out the methyl stearate that purity is 86%, stearic acid
The yield of methyl esters is 90%.
Embodiment 9
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, keeps essence
It is 0.6KPa to evaporate tower tower pressure, and bottom temperature is 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, tower top outflow
Light component in SBM raffinates, tower reactor outflow methyl stearate pregnant solution, methyl stearate purity is 75%.
Methyl stearate pregnant solution is introduced into extraction tower, methyl stearate pregnant solution enters from tower top, N- methyl
Pyrrolidones enters from tower bottom, and 1-METHYLPYRROLIDONE is 3: 1 with methyl stearate mass ratio, extraction tower
Number of theoretical plate is 10 pieces, and extraction temperature is 40 DEG C, and after counter-current extraction, bottom of towe outflow purity is 88%
Methyl stearate, the yield of methyl stearate is 90%.
Although the embodiment of the present invention is described in detail above in conjunction with the embodiments,
It is pointed out that protection scope of the present invention is not limited to these specific embodiments, but by weighing
Sharp claim determines.Those skilled in the art can be in the technological thought and the scope of purport for not departing from the present invention
It is interior that these embodiments are carried out with appropriate change, and the embodiment after these changes is obviously also included within this
Within the protection domain of invention.
Claims (3)
1. the method for methyl stearate is extracted in a kind of benzoyl methane raffinate from stearic acid, it is characterised in that：
(1) it is evaporated under reduced pressure：Stearoyl benzoyl methane raffinate is introduced into vacuum rectification tower, vacuum rectification tower
Pressure 0.6KPa~10KPa, bottom temperature are 160 DEG C~200 DEG C, and vacuum rectification tower number of theoretical plate is 20 pieces
- 40 pieces, reflux ratio is 2~5, and after rectification under vacuum, tower top flows out the component than methyl stearate low boiling point,
Methyl stearate and heavy constituent are flowed out by bottom of towe；
(2) liquid-liquid extraction：Methyl stearate pregnant solution is introduced into extraction tower, extraction tower operation temperature is
20 DEG C~60 DEG C, extractant is 1~3 with methyl stearate pregnant solution mass ratio：1, methyl stearate pregnant solution
Entering from tower top, extractant enters from tower bottom, after counter-current extraction, bottom of towe outflow methyl stearate.
2. according to the method for claim 1, it is characterised in that：The extraction that described liquid-liquid extraction uses
Agent is sulfolane, 1-METHYLPYRROLIDONE；Extractant is 1~3 with solution quality ratio to be extracted：1.
3. method according to claim 1 or 2, it is characterised in that：Described liquid-liquid extraction is using extraction
Tower is taken, extraction tower number of theoretical plate is 8~12 pieces, and operation temperature is 20 DEG C~60 DEG C.
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| CN201610383201.3A CN107459455B (en) | 2016-06-02 | 2016-06-02 | Method for extracting methyl stearate from benzoyl methane stearate residual liquid |
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| CN201610383201.3A CN107459455B (en) | 2016-06-02 | 2016-06-02 | Method for extracting methyl stearate from benzoyl methane stearate residual liquid |
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