CN104784959B - A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system - Google Patents
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system Download PDFInfo
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- CN104784959B CN104784959B CN201510201608.5A CN201510201608A CN104784959B CN 104784959 B CN104784959 B CN 104784959B CN 201510201608 A CN201510201608 A CN 201510201608A CN 104784959 B CN104784959 B CN 104784959B
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Abstract
The present invention relates to a kind of decompression interval lateral line discharging rectification and purification peach aldehyde system, including the tower reactor being sequentially connected with from bottom to top, king-tower and condenser, the sidepiece of king-tower connects lateral line discharging device, the tower top of king-tower connects tower top drawing mechanism, whole system is connected with vacuum pump group by buffer surge tank, controls absolute pressure through vacuum pump group and is not more than 1kPa.Compared with prior art, the present invention solves the separation of industrial peach aldehyde and is difficult to remove the problems such as the impurity composition of trace in product, product fragrance is poor, rectification time length, yield are low, energy consumption is big, provide a kind of rectifier unit producing high-quality peach aldehyde, light component in tower top separation and Extraction raw material in the apparatus, side line extracts and obtains high-quality peach aldehyde product, device flexible operation, the distillation operation time is short, production efficiency is high, peach aldehyde yield is between 82 85%, peach aldehyde product purity is up to the light component not affecting fragrance in more than 99.2%, and product.
Description
Technical field
The present invention relates to peach aldehyde isolation technics, especially relate to a kind of decompression interval lateral line discharging rectification and purification peach aldehyde
System.
Background technology
Peach aldehyde, also known as α-heptyl--butyrolactone, Tetradecanal, be a kind of water white transparency extremely slightly yellow liquid, have
Strong Fructus Persicae fragrance, as one of the most frequently used lactone spice, by FEMA (U.S.'s flavorant and extract
Maker association) regard as GRAS (it is generally acknowledged safety), FEMA numbering 3091, and through FDA (U.S. food
And FAD) ratify to eat, peach aldehyde is listed in and be can be used for not being detrimental to health in food by European Council
Artificial flavour table in.Peach aldehyde Flos Osmanthi Fragrantis, jasmine, Fructus Gardeniae, Herba Convallariae, orange blossom, rose white, Syringa oblata Lindl.,
The fragrances such as lilium auratum lindle the most often use, is also configuration Fructus Persicae, Fructus Melo, Fructus Armeniacae Mume, Fructus Pruni, Fructus Pruni pseudocerasi, Flos Osmanthi Fragrantis etc.
The first-class raw material of food flavor.It is practically insoluble in water, is dissolved in ethanol and most of ordinary organic solvents, can be extensive
It is applied to daily chemical essence and edible essence.
At present, peach aldehyde uses synthetic method to obtain mostly, and in prior art, the primary synthetic methods about peach aldehyde is
With n-octyl alcohol and acrylic acid methyl ester. as raw material, under the effect of free-radical initiator di-tert-butyl peroxide, make the most pungent
Alcohol becomes free radical, then carries out additive reaction with acrylic acid methyl ester., generate α-heptyl--butyrolactone.The method is former
Material is easy to get, and response path is short, and yield is high, it is easy to industrialization, but owing to this reaction is free radical addition reaction, and
Reaction conversion ratio is the highest, so reacting in the product obtained containing substantial amounts of weight composition impurity.Qualified in order to obtain
The peach aldehyde product required, it is necessary to crude reaction is purified.At present, the method for peach aldehyde separating-purifying is mainly adopted
Use Conventional batch rectifier unit, but peach aldehyde atmospheric boiling point is 297 DEG C, and there is thermal sensitivity, when temperature is more than 180 DEG C
Time peach aldehyde will thermally decompose, so conventional rectification method yield is extremely low.Patent CN1255395C describes one
Rectification under vacuum purifies the method for peach aldehyde, and the method is tower top discharging.Owing to peach aldehyde is the intermediate species in synthesis crude product,
Tower top to obtain highly purified peach aldehyde, first step tower top elder generation extraction capryl alcohol, second step extraction interim fraction, the 3rd step
Extraction reprocessed products, the mass fraction of peach aldehyde contained by the reprocessed products of now extraction, already close to finished product, causes the damage of peach aldehyde
Losing big, the yield causing last whole technique is the highest, and always contains a small amount of light in the peach aldehyde product obtained
Composition impurity, product fragrance is poor.Patent CN202246491U describes a set of peach aldehyde rectifying device, this device
Mainly solve peach aldehyde and separate the equipment needing two set different structures, i.e. flash distillation plant and rectifier unit, but this device is also
Being to use tower top discharge method, whole process energy consumption is big, yield is low, the longest, and the low fragrance of product purity is poor.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and a kind of flexible operation is provided,
The distillation operation time is short, and production efficiency is high, and energy consumption is low, peach aldehyde yield between 82-85%, peach aldehyde product purity
Decompression interval lateral line discharging rectification and purification Fructus Persicae up to the light component not affecting fragrance in more than 99.2%, and product
Aldehyde system.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system, including the tower reactor being sequentially connected with from bottom to top, master
Tower and condenser, the sidepiece of described king-tower connects lateral line discharging device, and the tower top of described king-tower connects tower top and goes out
Material device, whole system is connected with vacuum pump group by buffer surge tank, controls absolute pressure through vacuum pump group little
In 1kPa.
Being also associated with falling-film reboiler in described tower reactor, the Matter Transfer pipeline connected is provided with Flow-rate adjustment dress
Putting, circular flow scope is 1m3/ h～4m3/h。
Described king-tower has four Jie Tajie, and often joint height is at 3-3.5 rice.
It is provided with lateral line discharging device at the second tower joint and the 3rd tower joint of king-tower.
Described lateral line discharging device includes liquid header, liquid distribution trough and Produced Liquid amount controller.
Wherein, liquid header is riser formula liquid header, catcher perforated area 30%～60%, rises gas
Length of tube is 80mm～150mm.Liquid distribution trough is calandria liquid distributors, and wherein distributed points is 141～212
Individual every square metre.Produced Liquid amount controller is by controlling the extraction time to control liquid extraction ratio.
It is filled with high efficiency separation filler in described king-tower, can be random packing, regular wire packing or regular ripple
Card filler.
Owing to, in this separation system, separating the material that after raw material carrys out autoreaction, flash distillation obtains.Containing big in raw material
Measure the light component with octanal, capryl alcohol, n-octyl, methyl gamma decalactone etc. as representative and composition and answer
Miscellaneous heavy constituent, wherein in raw material, target product peach aldehyde boiling point is in centre, so when rectification and purification, Fructus Persicae in tower
The concentration distribution of aldehyde is first to raise to reduce afterwards from the bottom up, i.e. there is a maximum concentration peach aldehyde middle part in tower
Point, this concentration point gradually moves toward tower top along with the minimizing of light component, finally arrives tower top, therefore, the present invention
When extraction peach aldehyde product, first from bis-Ta Jiecai, then from the 3rd Ta Jiecai, finally adopt from tower top.With existing
Technology is compared, and the present invention is light component in tower top separation and Extraction raw material, and side line extracts and obtains high-quality peach aldehyde product,
Device flexible operation, the distillation operation time is short, and production efficiency is high, and peach aldehyde yield is between 82-85%, and peach aldehyde produces
Product purity is up to the light composition impurity extraction peach aldehyde product not affecting fragrance in more than 99.6%, and product.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the gas chromatogram of the product that embodiment 2 gathers.
In figure, 1-raw material storage tank, 2-feeds centrifugal pump, 3-charging regulation valve, 4-tower reactor, 5-circular centrifugal pump,
6-circulates feed adjustment valve, 7-falling-film reboiler, 8-king-tower, 9-condenser, 10-Produced Liquid amount controller, 11-
Product is by flow container, 12-the first side take-off mass flow controllers, and 13-the first sideline product is by flow container, 14-the second side line
Produced Liquid amount controller, 15-the second sideline product is by flow container, 16-buffer surge tank, 17-vacuum pump group.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system, its structure is as it is shown in figure 1, include from bottom to top
Tower reactor 4, king-tower 8 and the condenser 9 being sequentially connected with, tower reactor 4 is connected with raw material storage tank 1, is connecting on pipeline
It is additionally provided with charging centrifugal pump 2 and charging regulation valve 3, in order to carry and to control the addition of material.Square tube in tower reactor 4
Cross Flange joint king-tower 8, be connected with falling-film reboiler 7 by pipeline bottom tower reactor 4, pipeline be provided with circulate from
Heart pump 5 and circulation feed adjustment valve 6, be 1m in order to circulate and to control mass flow3/ h～4m3/h。
King-tower 8 includes four tower joints that up/down perforation connects, and often joint height saves built with efficiently at 3-3.5 rice, tower
Separating filler, can be random packing, regular wire packing or regular corrugation plate filler.At the second tower joint and the 3rd
The top of tower joint is provided with lateral line discharging device, and lateral line discharging device includes liquid header, liquid distribution trough and extraction
Mass flow controllers.Wherein, liquid header is riser formula liquid header, catcher perforated area 30%～60%,
A length of 80mm～150mm of riser.Liquid distribution trough is calandria liquid distributors, and wherein distributed points is
141～212 every square metre.Produced Liquid amount controller is by controlling the extraction time to control liquid extraction ratio.
The second tower joint product that gather out of side line enters the first sideline product by flow container 13, and through the first side take-off
Mass flow controllers 12 controls flow, and the 3rd tower joint product that gather out of side line enters the second sideline product by flow container 15,
And controlling flow through the second side take-off mass flow controllers 14, side line device is by pipeline and buffer surge tank 16
It is connected.Tower top is connected by pipeline with condenser 9, and condenser 9 is connected with the extraction device arranged at tower top,
The light component of overhead extraction and product enter product and are controlled through Produced Liquid amount controller 10 by flow container 11, extraction flow
System, whole system is also connected with buffer surge tank 16, and buffer surge tank 16 is connected with vacuum pump group 17,
To ensure the vacustat of whole system, absolute pressure is not more than 1kPa.
Embodiment 1
It is 12 meters at tower height, in the rectifying column of a diameter of 500mm, wherein liquid header perforated area 40%,
The a length of 100mm of riser, the distributed points of liquid distribution trough is 208 every square metre, by charging centrifugal pump
Putting into 2000kg peach aldehyde crude product with charging regulation valve to tower reactor, in crude product, peach aldehyde content is 88.08%, wherein than Fructus Persicae
The low-boiling impurity content of aldehyde is 8.31%, and the impurity content higher than peach aldehyde boiling point is 3.61%, then starts cooling
Water system, starts vacuum pump group, when system reaches separation requirement desirable pressure, when both absolute pressure is equal to 1kPa,
Starting Matter Transfer centrifugal pump, regulation flow is 2.5m3/ h, make material in tower reactor by circulation feed adjustment valve and
In falling-film reboiler, circulation is got up, and is then passed through the conduction oil that temperature is 220 DEG C in falling-film reboiler.When tower has
During steam, full tower is kept to reflux 1 hour, when tower top temperature is stablized at about 90 DEG C, by extraction liquid measure
The light component of 1:1 extraction pressed by controller, after produced quantity reaches the 11% of total feed liquid, closes tower top sampling, keeps tower complete
Backflow, 4:1 extraction 1-5kg overhead product is pressed in every infinite reflux for 2 hours.Now temperature at the second tower joint side take-off
Stable when 125-135 DEG C, start to take peach aldehyde product by 4:1, when produced quantity reaches total feed liquid at the second tower joint
30% time be switched to the 3rd tower joint side line by 4:1 extraction at, reach total when the 3rd tower saves produced quantity at side take-off
Feed liquid 50% time close side take-off, finally press the varying reflux ratio remaining product of mode extraction of 2:1-8:1 at tower top
Product, until product quality begins to decline.Analysis result proves, product peach aldehyde content to 99.01%,
Yield is 85.24%.
Embodiment 2
Operating procedure is same as Example 1, and regulation circular flow is 1m3/ h, conduction oil temperature is 220 DEG C.Analyze knot
Fruit proves, product peach aldehyde content is to 99.23%, and yield is 86%, and Fig. 2 is the gas phase color of the product gathered
Spectrogram, does not as can be seen from the figure have miscellaneous peak before peach aldehyde peak, say, that do not have light component in this sample.Peach aldehyde
There are two little miscellaneous peaks after peak, but content is extremely low, and heavy constituent is not the biggest on the impact of peach aldehyde fragrance.Can obtain as
The peach aldehyde product of this content, is that the content of peach aldehyde concentration is relatively simultaneously owing to lateral line discharging position does not has light component substantially
High.
Embodiment 3
Operating procedure is same as Example 1, and regulation circular flow is 4m3/ h, conduction oil temperature is 240 DEG C.Analyze knot
Fruit proves, product peach aldehyde content is to 98.71%, and yield is 81.35%
Embodiment 4
Tower height is 12 meters, in the rectifying column of a diameter of 500mm, and wherein liquid header perforated area 60%,
The a length of 100mm of riser, the distributed points of liquid distribution trough is 141 every square metre, by charging centrifugal pump
Putting into 2000kg peach aldehyde crude product with charging regulation valve to tower reactor, in crude product, peach aldehyde content is 88.08%, wherein than Fructus Persicae
The low-boiling impurity content of aldehyde is 8.31%, and the impurity content higher than peach aldehyde boiling point is 3.61%, then starts cooling
Water system, starts vacuum pump group, when system reaches separation requirement desirable pressure, when i.e. absolute pressure is equal to 1kPa,
Starting Matter Transfer centrifugal pump, regulation flow is 2.5m3/ h, make material in tower reactor by circulation feed adjustment valve and
In falling-film reboiler, circulation is got up, and is then passed through the conduction oil that temperature is 220 DEG C in falling-film reboiler.When tower has
During steam, full tower is kept to reflux 1 hour, when tower top temperature is stablized at about 90 DEG C, by extraction liquid measure
The light component of 1:1 extraction pressed by controller, after produced quantity reaches the 11% of total feed liquid, closes tower top sampling, keeps tower complete
Backflow, 4:1 extraction 1-5kg overhead product is pressed in every infinite reflux for 2 hours.Now temperature at the second tower joint side take-off
Stable when 125-135 DEG C, start to take peach aldehyde product by 2:1, when produced quantity reaches total feed liquid at the second tower joint
30% time be switched to the 3rd tower joint side line by 2:1 extraction at, reach total when the 3rd tower saves produced quantity at side take-off
Feed liquid 50% time close side take-off, finally press the varying reflux ratio remaining product of mode extraction of 2:1-8:1 at tower top
Product, until product quality begins to decline.Analysis result proves, product peach aldehyde content to 98.91%,
Yield is 83.35%.
Embodiment 5
Operating procedure is same as Example 4, wherein liquid header perforated area 30%, a length of 100mm of riser,
The distributed points of liquid distribution trough is 212 every square metre.Analysis result proves, product peach aldehyde content is to arriving
99.11%, yield is 85.64%.
Embodiment 6
Operating procedure is same as Example 4, wherein liquid header perforated area 60%, a length of 150mm of riser,
The distributed points of liquid distribution trough is 212 every square metre, and circular flow is 4m3/h.Analysis result proves, product
Peach aldehyde content is to 98.66%, and yield is 80.14%.
Claims (7)
1. a decompression interval lateral line discharging rectification and purification peach aldehyde system, it is characterised in that under this system includes certainly
Tower reactor, king-tower and the condenser being sequentially connected with on and, the sidepiece of described king-tower connects lateral line discharging device, described
The tower top of king-tower connect tower top drawing mechanism, whole system is connected with vacuum pump group by buffer surge tank, and warp is very
Empty pump group controls absolute pressure and is not more than 1kPa；
Being also associated with falling-film reboiler in described tower reactor, the Matter Transfer pipeline connected is provided with Flow-rate adjustment dress
Putting, circular flow scope is 1m3/ h～4m3/ h, described king-tower has four Jie Tajie, and often joint height is at 3-3.5
Rice, is provided with lateral line discharging device at the second tower joint and the 3rd tower joint of king-tower.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 1, its feature
Being, described lateral line discharging device includes liquid header, liquid distribution trough and Produced Liquid amount controller.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 2, its feature
Being, described liquid header is riser formula liquid header, catcher perforated area 30%～60%, rises
Air tubing length is 80mm～150mm.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 2, its feature
Being, described liquid distribution trough is calandria liquid distributors, and wherein distributed points is 141～212 every square metre.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 2, its feature
Being, described Produced Liquid amount controller is by controlling the extraction time to control liquid extraction ratio.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 1, its feature
It is, in described king-tower, is filled with high efficiency separation filler.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system the most according to claim 6, its feature
Being, described high efficiency separation filler is random packing, regular wire packing or regular corrugation plate filler.
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| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN107337656B (en) * | 2017-08-09 | 2021-08-27 | 上海化工研究院有限公司 | Reaction system and method for continuously preparing gamma-undecalactone |
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| DE3938121A1 (en) * | 1989-11-16 | 1991-05-23 | Basf Ag | METHOD FOR SEPARATING (ALPHA) -BUTYROLACTONE FROM MIXTURES CONTAINING AMBER OF ACID ETHYL ETHER |
| CN201094869Y (en) * | 2007-09-24 | 2008-08-06 | 上海益民化工有限公司 | Multipurpose internal reflux distillation device |
| CN102309865B (en) * | 2011-09-08 | 2014-06-04 | 中国石油天然气集团公司 | Refining system for circulating 1, 3-propanediol in continuous production of poly(trimethylene terephthalate) |
| CN202554979U (en) * | 2012-04-05 | 2012-11-28 | 南京师范大学 | Side discharging type reduced-pressure rectifying device |
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