CN107459456A - 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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- CN107459456A CN107459456A CN201610387068.9A CN201610387068A CN107459456A CN 107459456 A CN107459456 A CN 107459456A CN 201610387068 A CN201610387068 A CN 201610387068A CN 107459456 A CN107459456 A CN 107459456A
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- Prior art keywords
- methyl stearate
- tower
- raffinate
- molecular distillation
- sbm
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The present invention relates to 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 passes through molecular distillation again.This method can from stearic acid benzoyl raffinate isolated purity more than 88% methyl stearate, while yield can reach more than 95%.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 extracts stearic acid from stearic acid benzoyl methane raffinate
The method of methyl esters.
Background technology
The production method of stearoyl benzoyl methane (SBM), it is by contracting by acetophenone, methyl stearate and sodium methoxide
Close, be acidified, after concentration step, obtained solid crude product is dissolved in recrystallisation solvent and crystallized, the crystallization production that will filter out
Stearoyl benzoyl methane product is obtained after thing drying.Stearoyl benzoyl methane (SBM) raffinate be in SBM production processes,
After Crystallization Separation product, raffinate of the mother liquor through being distilled to recover remained by solvent, the content about 60% of methyl stearate in raffinate, but
It is SBM raffinate complicated components, big multi-component boiling point is higher, it is difficult to isolate methyl stearate therein.Patent
CN201210332441 discloses a kind of method that methyl stearate is extracted in raffinate from SBM, the side crystallized using methanol extraction
Method is from SBM raffinates, but the content of methyl stearate that its extraction obtains is relatively low, because its process is more complicated, methyl stearate
Yield it 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, it is proposed that
The method that a kind of rectification under vacuum and molecular distillation are combined, methyl stearate is separated from SBM raffinates.SBM raffinates composition is complicated,
Boiling point is close, at relatively high temperatures can coking, emphasis of the present invention keeps relatively low temperature during methyl stearate is separated,
Therefore using the methyl stearate in the method enrichment SBM raffinates of rectification under vacuum, purity is subsequently obtained using molecule rectification process
Higher methyl stearate.This method technique is simple, easy to operate, can from SBM raffinates DNA purity be more than 88% it is hard
Resin acid methyl esters, while yield can reach more than 95%.
Technical scheme proposed by the present invention is：
(1) stearoyl benzoyl methane raffinate is introduced into vacuum rectification tower, rectification under vacuum pressure tower be 0.6KPa~
10KPa, vacuum rectification tower number of theoretical plate are 20~40 pieces, and reflux ratio is 2~5, and after rectification under vacuum, stearic acid is compared in tower top outflow
The component of methyl esters low boiling point, methyl stearate and heavy constituent are flowed out by bottom of towe；
(2) methyl stearate pregnant solution being introduced into molecular distillation apparatus, the pressure of molecular distillation apparatus is 10~30Pa, point
It is 105~125 DEG C from vapo(u)rizing temperature, collects the light component in molecular distillation apparatus, as methyl stearate.
In above-mentioned technical proposal, rectification under vacuum pressure tower 0.6KPa~10KPa, vacuum rectification tower number of theoretical plate is 20~40
Block, reflux ratio are 2~5, and bottom temperature is 160 DEG C~200 DEG C.
In above-mentioned technical proposal, described molecular distillation pressure is 10~30Pa, and vapo(u)rizing temperature is 105 DEG C~125 DEG C.
SBM raffinates are introduced into vacuum rectification tower, after rectification under vacuum, tower top flows out the group than methyl stearate low boiling point
Point, methyl stearate and heavy constituent are flowed out by bottom of towe.Bottom stream by molecular distillation, isolates purity up to more than 88% again
Methyl stearate.
Specifically, it is as follows to be evaporated under reduced pressure the step of separating SBM raffinates with the method that molecular distillation is combined：SBM is residual
Liquid is introduced into vacuum rectification tower, and vacuum rectification tower number of theoretical plate is more than 20 pieces, keep rectifying tower pressure for 0.6KPa~
10KPa, bottom temperature are 160 DEG C~200 DEG C, and reflux ratio is 2~5, light in tower top outflow SBM raffinates by being evaporated under reduced pressure
Component, tower reactor outflow methyl stearate pregnant solution.Methyl stearate pregnant solution is introduced into molecular distillation apparatus, molecular distillation apparatus
Pressure be 10~30Pa, separation vapo(u)rizing temperature is 105~125 DEG C, collects the light component in molecular distillation apparatus, as purity
For more than 88% methyl stearate.
Beneficial effect
SBM raffinates composition is complicated, and boiling point is close, and most of component boiling point is higher, at relatively high temperatures can coking, using subtracting
Pressure rectifying carries out methyl stearate and is enriched with the relative volatility that on the one hand can be improved between separate substance, is advantageous to methyl stearate
Enrichment, while during rectification under vacuum, tower reactor operation temperature is relatively low, can prevent the coking of high boiling substance.Stearic acid first
Ester pregnant solution extracts methyl stearate by molecule rectifying, on the one hand can reduce the possibility of high boiling substance coking, on the one hand
Recovery can be improved and obtain the purity and yield of methyl stearate.Compared with prior art, the advantage of the invention is that using decompression
The technique being combined with molecular distillation is distilled, technique is simple, easy to operate, can obtain purity from stearoyl benzoyl methane raffinate
Higher methyl stearate.
Embodiment
The embodiment of the present invention is described in detail below, it should be noted however that the protection of the present invention
Scope 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, and holding rectifying tower pressure is
0.6KPa, bottom temperature are 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, and tower reactor
Methyl stearate pregnant solution is flowed out, methyl stearate purity is 75%.Methyl stearate pregnant solution is introduced into molecular distillation apparatus,
The pressure of molecular distillation is 10Pa, and temperature is 105 DEG C, collects the light component that molecular distillation apparatus comes out, and produces purity as 90%
Methyl stearate, the yield of methyl stearate is 95%.
Embodiment 2
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, and holding rectifying tower pressure is
10KPa, bottom temperature are 200 DEG C, reflux ratio 5, by being evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, and tower reactor stream
Go out methyl stearate pregnant solution, methyl stearate purity is 75%.Methyl stearate pregnant solution is introduced into molecular distillation apparatus, point
The pressure of son distillation is 10Pa, and temperature is 105 DEG C, collects the light component that molecular distillation apparatus comes out, and it is 90% to produce purity
Methyl stearate, the yield of methyl stearate is 95%.
Embodiment 3
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, and holding rectifying tower pressure is
0.6KPa, bottom temperature are 160 DEG C, reflux ratio 2, by being evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, and tower reactor
Methyl stearate pregnant solution is flowed out, methyl stearate purity is 73%.Methyl stearate pregnant solution is introduced into molecular distillation apparatus,
The pressure of molecular distillation is 10Pa, and temperature is 105 DEG C, collects the light component that molecular distillation apparatus comes out, and produces purity as 88%
Methyl stearate, the yield of methyl stearate is 95%.
Embodiment 4
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 20 pieces, and holding rectifying tower pressure is
0.6KPa, bottom temperature are 160 DEG C, reflux ratio 5, by being evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, and tower reactor
Methyl stearate pregnant solution is flowed out, methyl stearate purity is 75%.Methyl stearate pregnant solution is introduced into molecular distillation apparatus,
The pressure of molecular distillation is 30Pa, and temperature is 125 DEG C, collects the light component that molecular distillation apparatus comes out, and produces purity as 90%
Methyl stearate, the yield of methyl stearate is 95%.
Embodiment 5
SBM raffinates are introduced into vacuum rectification tower, vacuum rectification tower number of theoretical plate is 40 pieces, and holding rectifying tower pressure is
10KPa, bottom temperature are 200 DEG C, reflux ratio 3, by being evaporated under reduced pressure, the light component in tower top outflow SBM raffinates, and tower reactor stream
Go out methyl stearate pregnant solution, methyl stearate purity is 75%.Methyl stearate pregnant solution is introduced into molecular distillation apparatus, point
The pressure of son distillation is 30Pa, and temperature is 125 DEG C, collects the light component that molecular distillation apparatus comes out, and it is 90% to produce purity
Methyl stearate, the yield of methyl stearate is 95%.
Although the embodiment of the present invention is described in detail above in conjunction with the embodiments, need to refer to
Go out, protection scope of the present invention is not limited to these specific embodiments, but is determined by claims.This
Art personnel can carry out appropriate in the range of the technological thought of the present invention and purport is not departed to these embodiments
Change, and the embodiment after these changes is obviously also included within protection scope of the present 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) stearoyl benzoyl methane raffinate being introduced into vacuum rectification tower, rectification under vacuum pressure tower is 0.6KPa~10KPa,
Vacuum rectification tower number of theoretical plate is 20~40 pieces, and reflux ratio is 2~5, and 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；
(2) methyl stearate pregnant solution is introduced into molecular distillation apparatus, the pressure of molecular distillation apparatus is 10~30Pa, and separation is steamed
Temperature is evaporated for 105~125 DEG C, collects the light component in molecular distillation apparatus, as methyl stearate.
2. according to the method for claim 1, it is characterised in that：Described rectification under vacuum pressure tower 0.6KPa~10KPa, subtracts
It is 20~40 pieces to press rectifying column number of theoretical plate, and reflux ratio is 2~5, and bottom temperature is 160 DEG C~200 DEG C.
3. method according to claim 1 or 2, it is characterised in that：Described molecular distillation pressure is 10~30Pa, distillation
Temperature is 105 DEG C~125 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610387068.9A CN107459456B (en) | 2016-06-02 | 2016-06-02 | Method for extracting methyl stearate from benzoyl methane stearate residual liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610387068.9A CN107459456B (en) | 2016-06-02 | 2016-06-02 | Method for extracting methyl stearate from benzoyl methane stearate residual liquid |
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| CN107459456A true CN107459456A (en) | 2017-12-12 |
| CN107459456B CN107459456B (en) | 2020-09-22 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837182A (en) * | 2005-12-30 | 2006-09-27 | 安阳化学工业集团有限责任公司 | Process for preparing alpha-ethyl linolenate with purity more than 80% |
| CN101139289A (en) * | 2007-08-22 | 2008-03-12 | 安阳化学工业集团有限责任公司 | Technique for producing alpha-linolenic acid ethyl with 90 percent more purity |
| CN102898303A (en) * | 2012-09-11 | 2013-01-30 | 安徽佳先功能助剂股份有限公司 | Method for extracting methyl stearate from stearoylbenzoylmethane raffinate |
| CN104086412A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Process method for producing butyl oleate by using rape oil fatty acid |
| CN104479883A (en) * | 2014-11-18 | 2015-04-01 | 青岛澳海生物有限公司 | Preparation method for fatty glyceride |
| CN106117050A (en) * | 2016-06-24 | 2016-11-16 | 四川欣美加生物医药有限公司 | Improve the method for the purity of EPA-E in fish oil |
-
2016
- 2016-06-02 CN CN201610387068.9A patent/CN107459456B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837182A (en) * | 2005-12-30 | 2006-09-27 | 安阳化学工业集团有限责任公司 | Process for preparing alpha-ethyl linolenate with purity more than 80% |
| CN101139289A (en) * | 2007-08-22 | 2008-03-12 | 安阳化学工业集团有限责任公司 | Technique for producing alpha-linolenic acid ethyl with 90 percent more purity |
| CN102898303A (en) * | 2012-09-11 | 2013-01-30 | 安徽佳先功能助剂股份有限公司 | Method for extracting methyl stearate from stearoylbenzoylmethane raffinate |
| CN104086412A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Process method for producing butyl oleate by using rape oil fatty acid |
| CN104479883A (en) * | 2014-11-18 | 2015-04-01 | 青岛澳海生物有限公司 | Preparation method for fatty glyceride |
| CN106117050A (en) * | 2016-06-24 | 2016-11-16 | 四川欣美加生物医药有限公司 | Improve the method for the purity of EPA-E in fish oil |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉花等: ""脂肪酸甲酯精制分离装置设计要点"", 《煤炭与化工》 * |
| 孙月娥等: ""分子蒸馏技术及其应用"", 《粮油加工》 * |
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