CN101514151B - Method for refining acetylacetone - Google Patents
Method for refining acetylacetone Download PDFInfo
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- CN101514151B CN101514151B CN2009100485001A CN200910048500A CN101514151B CN 101514151 B CN101514151 B CN 101514151B CN 2009100485001 A CN2009100485001 A CN 2009100485001A CN 200910048500 A CN200910048500 A CN 200910048500A CN 101514151 B CN101514151 B CN 101514151B
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- tower
- methyl ethyl
- ethyl diketone
- boiling
- acetylacetone
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Abstract
A method for refining high-purity acetylacetone comprises procedures of devolatiligation, deacidification and deanhydride to coarse acetylacetone which later on enters a refining tower T1. The method is characterized in that the refining tower T1 is a pressure relief refining tower, the high-purity acetylacetone is extracted from the upper side line of the rectification section in liquid phase, acetone generated by the decomposition of acetylacetone and low-boiling mixed components, such as isopropenyl acetate, which are not completely removed due to instability of the initial stage of the process, are collected at the top of the tower, returned to a coarse acetylacetone groove V1, placed in the refining tower T1 after the procedures of devolatiligation, deacidification and deanhydride, and the tower kettle uses high-boiling components. The invention has the advantages that the refining tower T1 has the function of removing a small mount of low-boiling components because of liquid phase side line discharge way thereof, meanwhile, the acetone and isopropenyl acetate obtained from the top of the tower can be recycled, and the tower kettle uses high-boiling components, so that the whole rectification section is easy to control, flexible in operation, high in purity of the finished products, and stable in mass content of 99.9%.
Description
Technical field
The present invention relates to a kind of chemical separating technology, particularly a kind of methyl ethyl diketone treating tower adopts the method for rectification under vacuum, side line discharge method continuous treating high-purity acetylacetone.
Background technology
Methyl ethyl diketone is a kind of important chemical and medicine intermediate; Can be used for synthetic sulfa drugs, fodder additives and catalyzer etc.; Development along with society; Purity requirement to methyl ethyl diketone is increasingly high, and the premium grads purity requirement reaches 99.9%, and this also has higher requirement to the continuous rectificating technique of methyl ethyl diketone.In the methyl ethyl diketone rectification working process, last treating tower adopts the mode of cat head extraction product, obtains methyl ethyl diketone at present.But in the actual production; Because the decomposes of methyl ethyl diketone produces acetone, perhaps since early stage the rectification working process instability cause isopropenyl acetate, the low component of boiling such as acetone, isopropenyl acetate gets in the last treating tower; And the treating tower of existing apparatus does not possess the function that removes the low component of boiling usually; In a single day therefore there is the low component of boiling to get into treating tower, then has the low component of boiling of certain content in the product all the time, can't obtain desired high-purity acetylacetone product.
Japanese Patent JP63162645 and Chinese patent CN1850763A all adopt batch fractionating method to make methyl ethyl diketone; Batch fractionating is because throughput is low; Production cycle is long, and the shortcoming such as repeated relatively poor of quality product can't satisfy the requirement of large scale continuous prod; English Patent GB1354180 adopts fractionated method, changes vacuum tightness, extraction acetic acid, aceticanhydride and methyl ethyl diketone step by step, and this method not only can't realize serialization production, and the methyl ethyl diketone product purity is not high; English Patent GB838142 adopts the mode of two-tower rectification, and separating acetyl acetone still owing to fluctuation of operating conditions, in case there is the low component of boiling to get into treating tower, then can't remove fully continuously, and product purity can't stably reach 99.9%.
Summary of the invention
The objective of the invention is to overcome in the prior art because among the low component entering final refining tower T1 that boil such as acetone that the methyl ethyl diketone decomposition produces and isopropenyl acetate; Thereby can't obtain the shortcoming of high purity product; The continuous treating method of the reliable high-purity acetylacetone of a kind of stable operation is provided, but not only operate continuously, and also the finished product purity is high; Mass content reaches 99.9%, is applicable to large-scale commercial prodn.
For achieving the above object, the technical scheme of employing is the continuous treating method of high-purity acetylacetone; Comprise thick methyl ethyl diketone earlier through taking off the low operation of boiling, depickling, take off anhydridization process, get into treating tower T1; It is characterized in that: the side line liquid phase is extracted high-purity acetylacetone out on rectifying section top; Overhead collection is because the acetone that methyl ethyl diketone decompose to produce and because leading portion operation instability causes the low blending ingredients that boil such as isopropenyl acetate that do not remove fully, and returns thick methyl ethyl diketone groove V1; Through take off the low operation of boiling, depickling gets into treating tower T1 after taking off anhydridization process again, the tower still extraction high component of boiling.
In the technique scheme, treating tower T1 for the decompression treating tower, tower top pressure be gauge pressure-40～-90kPa; Reflux ratio is 5～12; Feed entrance point is for to count the 30th～40 block of theoretical tray from cat head, and side line extraction position is for to count the 5th～15 block of theoretical tray from cat head, 70～115 ℃ of tower top temperatures; Tower still temperature is 100～130 ℃, and side line is extracted 85～120 ℃ of temperature out.
Advantage of the present invention is: through treating tower T1 liquid phase side line discharging form; Make treating tower T1 possess and remove a small amount of function of hanging down the component of boiling; Overcome because methyl ethyl diketone decomposes the low components of boiling such as acetone that produce causes with leading portion operating mode instability among the low component entering final refining tower T1 that boils such as isopropenyl acetate, thereby can't obtain the shortcoming of high purity product, simultaneously; Acetone that cat head obtains and isopropenyl acetate can be recycled, the tower still extraction high component of boiling.Make whole rectifying workshop section be easier to control, turndown ratio is big, and the finished product purity is high, and mass content stably reaches 99.9%.
Description of drawings
Fig. 1 methyl ethyl diketone rectification flow.
T1 treating tower among the figure; The thick methyl ethyl diketone groove of V1; The refining tower height of the V2 component groove that boils; The low component groove that boils of V3 treating tower; V4 methyl ethyl diketone product groove; E1 makes with extra care Tata still reboiler; E 3 treating tower overhead condensers; E2 treating tower side line discharging condensing surface.
Embodiment
The treating tower T1 that adopts in the practical implementation is the decompression treating tower, and process is taken off the low operation of boiling earlier, anhydridization process is taken off in depickling for 50 blocks of theoretical trays, thick methyl ethyl diketone, gets into treating tower T1 again.
Comparative Examples is that prior art is from treating tower T1 cat head extraction method for product.
Embodiment adopts treating tower T1 side line liquid phase discharging method of the present invention to prepare high-purity acetylacetone; The low blending ingredients that boil such as the acetone of overhead collection and isopropenyl acetate; Return thick methyl ethyl diketone groove V1, and get into treating tower T1 once more, the tower still extraction high component of boiling as charge raw material.
Each material component is weight percentage among Comparative Examples and the embodiment.
Comparative Examples 1
Feed entrance point is for to count the 30th block of theoretical tray from cat head, and feed composition is: 98.4% methyl ethyl diketone, 0.3% acetone, 0.3% isopropenyl acetate, the 1% high component of boiling.
The treating tower operational condition is: tower top pressure is gauge pressure-63kPa, and reflux ratio 5, tower top temperature are 105 ℃, 123 ℃ of tower still temperature.
The rectifying result: from treating tower T1 cat head extraction product, product purity is 99.2%.
Comparative Examples 2
Owing to take off the low operation fluctuation of operating conditions that boils; It is refining that isopropenyl acetate gets into later process treating tower T1; Consisting of of the thick methyl ethyl diketone of charging: 97% methyl ethyl diketone, 0.3% acetone, 1.7% isopropenyl acetate, the 1% high component of boiling, feed entrance point is for to count the 35th block of theoretical tray from cat head.
Treating tower T1 operational condition is: tower top pressure is gauge pressure-86kPa, and reflux ratio 5, tower top temperature are 75 ℃, 101 ℃ of tower still temperature.
The rectifying result: from treating tower T1 cat head extraction product, product purity is 97.9%
Visible by Comparative Examples 1 and Comparative Examples 2 data, adopt the cat head discharge method, if contain acetone and isopropenyl acetate in the raw material, then there are acetone and isopropenyl acetate in the product all the time, can't remove fully, can't obtain high-purity methyl ethyl diketone of 99.9%.
Embodiment 1
Feed entrance point is for to count the 30th block of theoretical tray from cat head, and the thick methyl ethyl diketone component concentration of charging is with Comparative Examples 1.
The treating tower operational condition: tower top pressure is gauge pressure-63kPa, and reflux ratio 5, tower top temperature are 108 ℃, 125 ℃ of tower still temperature, and the methyl ethyl diketone side line is extracted 110 ℃ of temperature out.
The rectifying result: methyl ethyl diketone extraction position is for to count the 10th block of theoretical tray from treating tower T1 side line from cat head, and product purity is 99.9%.
Embodiment 2
Because leading portion fluctuation of operating conditions; Cause in the charging isopropenyl acetate to get among the treating tower T1; Feed entrance point is for to count the 35th block of theoretical tray from cat head, the consisting of of the thick methyl ethyl diketone of charging: 97.7% methyl ethyl diketone, 0.3% acetone, 1% isopropenyl acetate, the 1% high component of boiling.
Treating tower T1 operational condition is: tower top pressure is gauge pressure-86kPa, and reflux ratio 5, tower top temperature are 75 ℃, 104 ℃ of tower still temperature, and the methyl ethyl diketone side line is extracted 86 ℃ of temperature out.
Methyl ethyl diketone is from the extraction of treating tower T1 side line, and it is the 15th block of theoretical tray that the position is counted from cat head, and the rectifying result: product purity is 99.9%.
Embodiment 3
Feed entrance point is for to count the 32nd block of theoretical tray from cat head; Because methyl ethyl diketone decomposites the low component of boiling such as acetone and gets among the treating tower T1, the consisting of of the thick methyl ethyl diketone of charging: 97.7% methyl ethyl diketone, 1% acetone, 0.3% isopropenyl acetate, the 1% high component of boiling.
Treating tower T1 operational condition is: tower top pressure is gauge pressure-45kPa, and reflux ratio 8, tower top temperature are 113 ℃, 129 ℃ of tower still temperature, and the methyl ethyl diketone side line is extracted 117 ℃ of temperature out.
Methyl ethyl diketone is from the extraction of treating tower T1 side line, and it is the 9th block of theoretical tray that the position is counted from cat head, rectifying result: product purity 99.9%.
Embodiment 4
Because leading portion fluctuation of operating conditions; Cause fed with acetone and isopropenyl acetate content overproof; Each component concentration in the thick methyl ethyl diketone: 97% methyl ethyl diketone, 1% acetone, 1% isopropenyl acetate, the 1% high component of boiling, feed entrance point is for to count the 40th block of theoretical tray from cat head.
Treating tower T1 operational condition: tower top pressure is gauge pressure-63kPa, and reflux ratio 6, tower top temperature are 108 ℃, 125 ℃ of tower still temperature, and the methyl ethyl diketone side line is extracted 110 ℃ of temperature out.
Methyl ethyl diketone is from the extraction of treating tower T1 side line, and the position is counted to being the 8th block of theoretical tray from cat head, and the rectifying result: product purity is 99.9%.
Embodiment 5
Because the leading portion fluctuation of operating conditions is excessive; Cause acetone and isopropenyl acetate content severe overweight in the charging; Each component and content are respectively in the thick methyl ethyl diketone: the component charging of boiling of 94.5% methyl ethyl diketone, 2% acetone, 2.5% isopropenyl acetate, 1% height, feed entrance point is for to count the 38th block of theoretical tray from cat head.
The operational condition of treating tower T1: tower top pressure is gauge pressure-71kPa, and reflux ratio 12, tower top temperature are 85 ℃, 122 ℃ of tower still temperature, and the methyl ethyl diketone side line is extracted 101 ℃ of temperature out.
Methyl ethyl diketone is from the extraction of treating tower T1 side line, and the position is the 13rd a block of theoretical tray, and the rectifying result: product purity is 99.9%.
Can know by instance 3, instance 4 and instance 5,, make treating tower T1 possess and remove a small amount of function of hanging down the component of boiling through the mode of treating tower T1 liquid phase side line discharging.Even, cause a large amount of low components of boiling to get among the treating tower T1, finally still can obtain purity up to 99.9% methyl ethyl diketone product because leading portion fluctuation of operating conditions or methyl ethyl diketone decompose.Simultaneously, acetone that cat head obtains and isopropenyl acetate can be recycled, and return thick methyl ethyl diketone groove V1 once more as treating tower T1 charge raw material, the tower still extraction high component of boiling.
Claims (1)
1. the process for purification of a methyl ethyl diketone comprises thick methyl ethyl diketone earlier through taking off the low operation of boiling, and anhydridization process is taken off in depickling; Get into treating tower T1, it is characterized in that: the side line liquid phase is extracted high-purity acetylacetone out on rectifying section top, overhead collection low boil blending ingredients acetone and isopropenyl acetate; And return thick methyl ethyl diketone groove V1; Again through taking off the low operation of boiling, anhydridization process is taken off in depickling, gets into treating tower T1 then, the tower still extraction high component of boiling;
Said treating tower T1 is the decompression treating tower; Tower top pressure be gauge pressure-40～-90kPa, feed entrance point is for to count the 30th～40 block of theoretical tray from cat head, side line extraction position is for to count the 5th～15 block of theoretical tray from cat head; 70～115 ℃ of tower top temperatures; Tower still temperature is 100～130 ℃, and side line is extracted 85～120 ℃ of temperature, reflux ratio 5～12 out.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100485001A CN101514151B (en) | 2009-03-30 | 2009-03-30 | Method for refining acetylacetone |
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| CN2009100485001A CN101514151B (en) | 2009-03-30 | 2009-03-30 | Method for refining acetylacetone |
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| CN101514151A CN101514151A (en) | 2009-08-26 |
| CN101514151B true CN101514151B (en) | 2012-07-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB838142A (en) * | 1957-10-10 | 1960-06-22 | Courtaulds Ltd | Improvements in and relating to the production of acetyl acetone |
| US3794686A (en) * | 1970-09-25 | 1974-02-26 | Wacker Chemie Gmbh | Process for continuously producing acetylacetone |
| CN1850763A (en) * | 2006-05-25 | 2006-10-25 | 宁波王龙集团有限公司 | Process for preparing high-purity acetylacetone |
| CN101386572A (en) * | 2008-10-28 | 2009-03-18 | 上海吴泾化工有限公司 | Method for separating and purifying acetylacetone |
-
2009
- 2009-03-30 CN CN2009100485001A patent/CN101514151B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB838142A (en) * | 1957-10-10 | 1960-06-22 | Courtaulds Ltd | Improvements in and relating to the production of acetyl acetone |
| US3794686A (en) * | 1970-09-25 | 1974-02-26 | Wacker Chemie Gmbh | Process for continuously producing acetylacetone |
| CN1850763A (en) * | 2006-05-25 | 2006-10-25 | 宁波王龙集团有限公司 | Process for preparing high-purity acetylacetone |
| CN101386572A (en) * | 2008-10-28 | 2009-03-18 | 上海吴泾化工有限公司 | Method for separating and purifying acetylacetone |
Non-Patent Citations (2)
| Title |
|---|
| JP昭63-162645A 1988.07.06 |
| 说明书附图. |
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