CN104784959A - System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification - Google Patents
System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification Download PDFInfo
- Publication number
- CN104784959A CN104784959A CN201510201608.5A CN201510201608A CN104784959A CN 104784959 A CN104784959 A CN 104784959A CN 201510201608 A CN201510201608 A CN 201510201608A CN 104784959 A CN104784959 A CN 104784959A
- Authority
- CN
- China
- Prior art keywords
- tower
- peach aldehyde
- rectification
- lateral line
- purification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a system for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification. The system comprises a tower kettle, a main tower and a condenser, which are connected in sequence from the bottom to top, wherein the side part of the main tower is connected with a side withdrawal device; the tower top of the main tower is connected with a tower top discharging device; the whole system is connected with a vacuum pump group through a buffer tank; through the vacuum pump group, the absolute pressure is not greater than 1 kPa. Compared with the prior art, the system provided by the invention is capable of solving the problems that the micro impurity components in the product are difficult to remove in the industrial peach aldehyde separation and the product is bad in fragrance, long in rectification time, low in yield and large in energy consumption, and a rectification device for producing high-quality peach aldehyde is provided; according to the device, tower top separation is carried out to extract the light components in the raw materials and side extraction is carried out to obtain high-quality peach aldehyde products; the device is flexible to operate, short in rectification operation time and high in production efficiency; the peach aldehyde yield is within 82-85%, the purity of the peach aldehyde product is 99.2% or above and the product does not contain light components which influence the fragrance.
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, undecalactone, that a kind of water white transparency is to micro-yellow liquid, there is strong peach fragrance, as one of the most frequently used lactone spice, GRAS (it is generally acknowledged safety) is regarded as by FEMA (U.S.'s flavorant and extract producer association), FEMA numbering 3091, and edible through FDA (U.S. food and FAD) approval, and peach aldehyde is listed in the artificial flavour table that can be used for not being detrimental to health in food by European Council.Peach aldehyde all often uses in the fragrances such as sweet osmanthus, jasmine, cape jasmine, the lily of the valley, flores aurantii, rose white, lilac, lilium auratum lindle, is also the first-class raw material of the food flavors such as configuration peach, muskmelon, plum, apricot, cherry, sweet osmanthus.Water-soluble hardly, be dissolved in ethanol and most of OOS, daily chemical essence and flavoring essence can be widely used in.
At present, peach aldehyde adopts synthetic method to obtain mostly, in prior art, primary synthetic methods about peach aldehyde is for raw material with n-octyl alcohol and methyl acrylate, under the effect of free-radical initiator di-tert-butyl peroxide, make n-octyl alcohol become free radical, then carry out addition reaction with methyl acrylate, generation α-heptyl-
-butyrolactone.The method raw material is easy to get, and response path is short, and yield is high, is easy to industrialization, but due to this reaction be free radical addition reaction, and reaction conversion ratio is not high, so containing a large amount of weight composition impurities in the product be obtained by reacting.In order to obtain the peach aldehyde product of Eligibility requirements, must purify to crude reaction.At present, the method for peach aldehyde separating-purifying mainly adopts Conventional batch rectifier unit, but peach aldehyde atmospheric boiling point is 297 DEG C, and has thermal sensitivity, and when temperature is more than 180 DEG C, peach aldehyde will thermal decomposition, so conventional rectification method yield is extremely low.Patent CN1255395C describes a kind of method of rectification under vacuum purification peach aldehyde, and the method is tower top discharging.Due to the intermediate species that peach aldehyde is in synthesis crude product, tower top will obtain highly purified peach aldehyde, the first extraction octanol of first step tower top, second step extraction interim fraction, the 3rd step extraction reprocessed products, contained by the reprocessed products of now extraction, the mass fraction of peach aldehyde is close to finished product, cause the loss of peach aldehyde large, cause a yield of last whole technique not high, and always containing a small amount of light component impurity in the peach aldehyde product obtained, product fragrance is poor.Patent CN202246491U describes a set of peach aldehyde rectifying device, this device mainly solves peach aldehyde and is separated the equipment that needs two overlap different structure, i.e. flash distillation plant and rectifier unit, but this device still adopts tower top discharge method, whole process energy consumption is large, yield is low, length consuming time, and the low fragrance of product purity is poor.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of flexible operation is provided, the distillation operation time is short, production efficiency is high, energy consumption is low, peach aldehyde yield is between 82-85%, peach aldehyde product purity can reach more than 99.2%, and does not affect the decompression interval lateral line discharging rectification and purification peach aldehyde system of the light component of fragrance in product.
Object 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, comprise the tower reactor, king-tower and the condenser that connect successively from bottom to top, the sidepiece of described king-tower connects side line drawing mechanism, the tower top of described king-tower connects tower top drawing mechanism, whole system is connected with vavuum pump group by buffer surge tank, controls absolute pressure be not more than 1kPa through vavuum pump group.
Described tower reactor is also connected with falling-film reboiler, and the Matter Transfer pipeline connected is provided with flow regulator, and circular flow scope is 1m
3/ h ~ 4m
3/ h.
Described king-tower has four Jie Tajie, and often joint height is at 3-3.5 rice.
King-tower second tower joint and the 3rd tower joint place be provided with lateral line discharging device.
Described lateral line discharging device comprises liquid header, liquid distribution trough and Produced Liquid amount controller.
Wherein, liquid header is riser formula liquid header, collector perforated area 30% ~ 60%, and riser length is 80mm ~ 150mm.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.
Being filled with efficient separating filler in described king-tower, can be random packing, regular wire packing or regular corrugation plate filler.
Due in this separation system, the material that after separate raw materials carrys out autoreaction, flash distillation obtains.Contain a large amount of with octanal in raw material, octanol, n-octyl, methyl gamma decalactones etc. are the light component of representative and the heavy constituent of composition and complexity thereof, in its Raw, target product peach aldehyde boiling point mediates, so when rectification and purification, in tower, the CONCENTRATION DISTRIBUTION of peach aldehyde is first raise rear reduction from the bottom up, namely there is a maximum concentration point middle part of peach aldehyde in tower, this concentration point moves toward tower top gradually along with the minimizing of light component, finally arrive tower top, therefore, the present invention is when extraction peach aldehyde product, first from bis-Ta Jiecai, then from the 3rd Ta Jiecai, finally adopt from tower top.Compared with prior art, the present invention is light component in tower top separation and Extraction raw material, 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%, peach aldehyde product purity can reach more than 99.6%, and does not affect the light component impurity extraction peach aldehyde product of fragrance in product.
Accompanying drawing explanation
Fig. 1 is 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 in raw material centrifugal pump, 3-feeds in raw material control valve, 4-tower reactor, 5-circular centrifugal pump, 6-circulation feed liquid control valve, 7-falling-film reboiler, 8-king-tower, 9-condenser, 10-Produced Liquid amount controller, 11-product is by flow container, 12-first side take-off mass flow controllers, 13-first sideline product is subject to flow container, 14-second side take-off mass flow controllers, 15-second sideline product is subject to flow container, 16-buffer surge tank, 17-vavuum pump group.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system, its structure as shown in Figure 1, comprise the tower reactor 4, king-tower 8 and the condenser 9 that connect successively from bottom to top, tower reactor 4 is connected with raw material storage tank 1, connecting pipe is also provided with reinforced centrifugal pump 2 and reinforced control valve 3, in order to adding of transmission and control material.By Flange joint king-tower 8 above tower reactor 4, be connected with falling-film reboiler 7 by pipeline bottom tower reactor 4, pipeline is provided with circular centrifugal pump 5 and circulation feed liquid control valve 6, is 1m in order to circulation and control mass flow
3/ h ~ 4m
3/ h.
King-tower 8 comprises four tower joints that up/down perforation connects, and often joint height is at 3-3.5 rice, and tower joint, built with efficient separating filler, can be random packing, regular wire packing or regular corrugation plate filler.Be provided with lateral line discharging device at the top of the second tower joint and the 3rd tower joint, lateral line discharging device comprises liquid header, liquid distribution trough and Produced Liquid amount controller.Wherein, liquid header is riser formula liquid header, collector perforated area 30% ~ 60%, and riser length is 80mm ~ 150mm.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.
Product introduction first sideline product that second tower joint side line gathers out is by flow container 13, and control flow through the first side take-off mass flow controllers 12, product introduction second sideline product that 3rd tower joint side line gathers out is by flow container 15, and controlling flow through the second side take-off mass flow controllers 14, side line device is connected with buffer surge tank 16 by pipeline.Tower top is connected by pipeline with condenser 9, the extraction device that condenser 9 and tower top place are arranged is connected, overhead extraction light component and product introduction product are by flow container 11, extraction flow controls through Produced Liquid amount controller 10, whole system is also connected with buffer surge tank 16, buffer surge tank 16 is connected with vavuum pump group 17, and to ensure the vacustat of whole system, absolute pressure is not more than 1kPa.
Embodiment 1
It is 12 meters at tower height, diameter is in the rectifying column of 500mm, wherein liquid header perforated area 40%, riser length is 100mm, the distributed points of liquid distribution trough is 208 every square metre, 2000kg peach aldehyde crude product is dropped into tower reactor by charging centrifugal pump and charging control valve, in crude product, peach aldehyde content is 88.08%, be wherein 8.31% than the low-boiling impurity content of peach aldehyde, the impurity content higher than peach aldehyde boiling point is 3.61%, then cooling water system is started, start vavuum pump group, when system reaches pressure needed for separation requirement, both when absolute pressure equals 1kPa, start Matter Transfer centrifugal pump, adjust flux is 2.5m
3/ h, makes material circulate in tower reactor and falling-film reboiler by circulation feed liquid control valve, then in falling-film reboiler, passes into the conduction oil that temperature is 220 DEG C.When tower has steam, full tower is kept to reflux 1 hour, when tower top temperature is stabilized in about 90 DEG C, 1:1 extraction light component is pressed by Produced Liquid amount controller, after produced quantity reaches 11% of total feed liquid, pass tower top sampling, keep tower infinite reflux, 4:1 extraction 1-5kg overhead product is pressed in every infinite reflux for 2 hours.Now the second tower joint side take-off place temperature stabilization is when 125-135 DEG C, start to take peach aldehyde product at the second tower joint by 4:1, the 3rd tower joint side line is switched to by 4:1 extraction place when produced quantity reaches 30% of total feed liquid, side take-off is closed when the 3rd tower joint side take-off place produced quantity reaches 50% of total feed liquid, the last remaining product of varying reflux ratio mode extraction pressing 2:1-8:1 at tower top, until product quality starts to decline.Analysis result proves, product peach aldehyde content is to 99.01%, and yield is 85.24%.
Embodiment 2
Operating procedure is same as Example 1, and adjustment circular flow is 1m
3/ h, conduction oil temperature is 220 DEG C.Analysis result proves, product peach aldehyde content is to 99.23%, and the gas chromatogram of yield to be 86%, Fig. 2 the be product gathered, as can be seen from the figure assorted peak before peach aldehyde peak, does not that is have light component in this sample.Have two little assorted peaks after peach aldehyde peak, but content is extremely low, and heavy constituent not very large on the impact of peach aldehyde fragrance.Can obtain the peach aldehyde product of content like this, be because lateral line discharging position does not have light component substantially, and the content of peach aldehyde concentration is higher simultaneously.
Embodiment 3
Operating procedure is same as Example 1, and adjustment circular flow is 4m
3/ h, conduction oil temperature is 240 DEG C.Analysis result proves, product peach aldehyde content is to 98.71%, and yield is 81.35%
Embodiment 4
Tower height is 12 meters, diameter is in the rectifying column of 500mm, wherein liquid header perforated area 60%, riser length is 100mm, the distributed points of liquid distribution trough is 141 every square metre, 2000kg peach aldehyde crude product is dropped into tower reactor by charging centrifugal pump and charging control valve, in crude product, peach aldehyde content is 88.08%, be wherein 8.31% than the low-boiling impurity content of peach aldehyde, the impurity content higher than peach aldehyde boiling point is 3.61%, then cooling water system is started, start vavuum pump group, when system reaches pressure needed for separation requirement, namely when absolute pressure equals 1kPa, start Matter Transfer centrifugal pump, adjust flux is 2.5m
3/ h, makes material circulate in tower reactor and falling-film reboiler by circulation feed liquid control valve, then in falling-film reboiler, passes into the conduction oil that temperature is 220 DEG C.When tower has steam, full tower is kept to reflux 1 hour, when tower top temperature is stabilized in about 90 DEG C, 1:1 extraction light component is pressed by Produced Liquid amount controller, after produced quantity reaches 11% of total feed liquid, pass tower top sampling, keep tower infinite reflux, 4:1 extraction 1-5kg overhead product is pressed in every infinite reflux for 2 hours.Now the second tower joint side take-off place temperature stabilization is when 125-135 DEG C, start to take peach aldehyde product at the second tower joint by 2:1, the 3rd tower joint side line is switched to by 2:1 extraction place when produced quantity reaches 30% of total feed liquid, side take-off is closed when the 3rd tower joint side take-off place produced quantity reaches 50% of total feed liquid, the last remaining product of varying reflux ratio mode extraction pressing 2:1-8:1 at tower top, until product quality starts to decline.Analysis result proves, product peach aldehyde content is to 98.91%, and yield is 83.35%.
Embodiment 5
Operating procedure is same as Example 4, wherein liquid header perforated area 30%, and riser length is 100mm, and the distributed points of liquid distribution trough is 212 every square metre.Analysis result proves, product peach aldehyde content is to 99.11%, and yield is 85.64%.
Embodiment 6
Operating procedure is same as Example 4, wherein liquid header perforated area 60%, and riser length is 150mm, and 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 (10)
1. a decompression interval lateral line discharging rectification and purification peach aldehyde system, it is characterized in that, this system comprises the tower reactor, king-tower and the condenser that connect successively from bottom to top, the sidepiece of described king-tower connects side line drawing mechanism, the tower top of described king-tower connects tower top drawing mechanism, whole system is connected with vavuum pump group by buffer surge tank, controls absolute pressure be not more than 1kPa through vavuum pump group.
2. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 1, it is characterized in that, described tower reactor is also connected with falling-film reboiler, the Matter Transfer pipeline connected is provided with flow regulator, and circular flow scope is 1m
3/ h ~ 4m
3/ h.
3. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 1, it is characterized in that, described king-tower has four Jie Tajie, and often joint height is at 3-3.5 rice.
4. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 3, is characterized in that, is provided with lateral line discharging device at the second tower joint of king-tower and the 3rd tower joint place.
5. the one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 1 or 4, it is characterized in that, described lateral line discharging device comprises liquid header, liquid distribution trough and Produced Liquid amount controller.
6. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 5, it is characterized in that, described liquid header is riser formula liquid header, collector perforated area 30% ~ 60%, and riser length is 80mm ~ 150mm.
7. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 5, it is characterized in that, described liquid distribution trough is calandria liquid distributors, and wherein distributed points is 141 ~ 212 every square metre.
8. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 5, it is characterized in that, described Produced Liquid amount controller is by controlling the extraction time to control liquid extraction ratio.
9. the one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 1 or 3 or 4, is characterized in that, be filled with efficient separating filler in described king-tower.
10. one decompression interval lateral line discharging rectification and purification peach aldehyde system according to claim 9, it is characterized in that, described efficient separating filler is random packing, regular wire packing or regular corrugation plate filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510201608.5A CN104784959B (en) | 2015-04-24 | 2015-04-24 | A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510201608.5A CN104784959B (en) | 2015-04-24 | 2015-04-24 | A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104784959A true CN104784959A (en) | 2015-07-22 |
| CN104784959B CN104784959B (en) | 2016-08-17 |
Family
ID=53550423
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510201608.5A Active CN104784959B (en) | 2015-04-24 | 2015-04-24 | A kind of decompression interval lateral line discharging rectification and purification peach aldehyde system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104784959B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN107337656A (en) * | 2017-08-09 | 2017-11-10 | 上海化工研究院有限公司 | A kind of continuous reaction system and method for preparing γ undecalactones |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5030328A (en) * | 1989-11-16 | 1991-07-09 | Basf Aktiengesellschaft | Method of separating γ-butyrolactone from mixtures containing diethyl succinate |
| CN201094869Y (en) * | 2007-09-24 | 2008-08-06 | 上海益民化工有限公司 | Multipurpose internal reflux distillation device |
| CN102309865A (en) * | 2011-09-08 | 2012-01-11 | 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 |
-
2015
- 2015-04-24 CN CN201510201608.5A patent/CN104784959B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5030328A (en) * | 1989-11-16 | 1991-07-09 | Basf Aktiengesellschaft | Method of separating γ-butyrolactone from mixtures containing diethyl succinate |
| CN201094869Y (en) * | 2007-09-24 | 2008-08-06 | 上海益民化工有限公司 | Multipurpose internal reflux distillation device |
| CN102309865A (en) * | 2011-09-08 | 2012-01-11 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN107337656A (en) * | 2017-08-09 | 2017-11-10 | 上海化工研究院有限公司 | A kind of continuous reaction system and method for preparing γ undecalactones |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104784959B (en) | 2016-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102504955B (en) | Processing for extracting and purifying eucalyptus oil | |
| CN105348098B (en) | Method for rectifying and separating methyl formate, methanol and water by intermittent reaction | |
| CN104784959A (en) | System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification | |
| CN101381273A (en) | Method for preparing isobutene by tert-butanol and apparatus | |
| CN100427468C (en) | Apparatus and method for separating 5-bromo-2-methyl pyridine isomer by intermittent rectification under vacuum | |
| CN109851499A (en) | A kind of method and device using benzene in azeotropic distillation separation vinylacetate | |
| CN107098797A (en) | A kind of extracting method of chavicol methyl ether | |
| CN104961624B (en) | Octyl alconyl produces the recoverying and utilizing method of waste liquid | |
| CN102091432B (en) | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device | |
| KR20180067562A (en) | Method for purifying methyl methacrylate | |
| CN202270376U (en) | Continuous rectifying device | |
| CN212818203U (en) | Separation and purification device for preparing watermelon ketone | |
| CN102391216B (en) | Peach aldehyde rectification equipment | |
| CN107188784A (en) | A kind of extracting method of linalool | |
| CN202246491U (en) | Peach aldehyde rectification device | |
| CN110357771A (en) | A kind of partition tower process of methyl lactate hydrolysis rectifying | |
| CN204111623U (en) | A kind of process unit of purifying for by product diisopropyl ether in Virahol production | |
| CN207375972U (en) | A kind of 1,10- decanediols continuous production system | |
| CN104177234B (en) | The refined purifying plant of a kind of by-product diisopropyl ether in isopropanol produces and method | |
| CN101830780A (en) | Method and device for separating mixed substances in reaction solution for oxidation of phenol with hydrogen peroxide | |
| CN105693754A (en) | Organosilicone high-boiling-component removing and low-boiling-component removing tower pressure-variable thermal coupling distillation method and equipment | |
| CN112386935A (en) | Method for separating acetic acid hydrogenation ethanol product by adopting dividing wall rectifying tower | |
| CN106187765B (en) | Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate | |
| CN101306982A (en) | Method for intermittently extracting, rectifying and separating ethanol and xylol mixture | |
| CN1456382A (en) | Packed tower top gas-liquid splite-flow reflux balancing distributing distilling producing process devics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 200062 Shanghai city Putuo District Yunling Road No. 345 Patentee after: Shanghai Chemical Research Institute Co., Ltd. Address before: 200062 Shanghai city Putuo District Yunling Road No. 345 Patentee before: Shanghai Research Institute of Chemical Industry |