CN1109861A - Rectifying device for refining crude vanillin - Google Patents
Rectifying device for refining crude vanillin Download PDFInfo
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- CN1109861A CN1109861A CN 95102143 CN95102143A CN1109861A CN 1109861 A CN1109861 A CN 1109861A CN 95102143 CN95102143 CN 95102143 CN 95102143 A CN95102143 A CN 95102143A CN 1109861 A CN1109861 A CN 1109861A
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- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The rectifying equipment for refining crude vanillin is composed of specially designed efficient rectifying tower, tower still with cold storage function, circulating pump of tower still, falling-film reboiler, condensater, built-in reflux ratio controller and storage tanks, and features its simplified technology.
Description
The present invention relates to a kind of rectifier unit that is used for refining crude vanillin, international Patent classificating number is CO7C47/58.
Vanillin food grade,1000.000000ine mesh (chemical name is a 4-hydroxyl 3-methoxybenzaldehyde) is that a kind of consumption is big, the spices that purposes is wide.Be widely used in candy, cake, food flavor(ing) and health product such as alcoholic drink mixed with fruit juice in the cosmetic essence, also are used for pharmacy, tanning, rubber item is in the industries such as plating.
Synthesis of vanillin adopts the methyl catechol route usually.Generate vanillin food grade,1000.000000ine mesh by methyl catechol (hydroxyanisole) and formaldehyde condensation.The synthetic vanillin food grade,1000.000000ine mesh extracts with benzene, obtains the vanillin food grade,1000.000000ine mesh raw product after benzene is steamed.The vanillin food grade,1000.000000ine mesh raw product contains the ortho vanillin (4-hydroxyl 2-methoxybenzaldehyde) about 5% approximately, a small amount of light constituent, 70～80% vanillin food grade,1000.000000ine meshs and heavy constituent-tar of about 20%.The separation and purification process is the vanillin food grade,1000.000000ine mesh raw product, purifies to food grade vanillin food grade,1000.000000ine mesh finished product.
Usually the separation method that adopts is that the vanillin food grade,1000.000000ine mesh raw product is added common still kettle, the simple distillation of reducing pressure, and vanillin food grade,1000.000000ine mesh, ortho vanillin and a small amount of heavy constituent steam from still.Stay heavy constituent impurity-tar at the bottom of the still.The material toluene that steams is that solvent carries out crystallization, mainly is ortho vanillin and vanillin food grade,1000.000000ine mesh are separated.The vanillin food grade,1000.000000ine mesh primary product that crystallization obtains adds in second still kettle again, and the heavy constituent impurity in the vanillin food grade,1000.000000ine mesh is removed in the simple distillation of reducing pressure again, obtains the vanillin food grade,1000.000000ine mesh product.
Vanillin food grade,1000.000000ine mesh is the high-solidification point heat-sensitive substance, meets oxygen and easily be oxidized to acid in still-process, and high-temperature heating easily produces polymerization.The oxypolymerization of vanillin food grade,1000.000000ine mesh in still-process all can cause the vanillin food grade,1000.000000ine mesh yield to reduce.Vanillin food grade,1000.000000ine mesh is a kind of high value product, reduces loss in the sepn process and be one of key that factory increases economic efficiency, and above-mentioned separation method adopts twice underpressure distillation and a toluene crystallization separation process that many shortcomings are arranged.At first, adopt the method for simple still distillation, because simple distillation has only one to separate level, separation efficiency is poor, is difficult to each component is thoroughly separated.So adopt twice simple distillation in the former technology, its purpose all is for the heavy constituent tar separation.Because the boiling point of vanillin food grade,1000.000000ine mesh and its isomer is more approaching, adopt simple distillation ortho vanillin can't be separated well with the contraposition vanillin food grade,1000.000000ine mesh, have to adopt toluene crystalline method to separate contraposition vanillin food grade,1000.000000ine mesh and ortho vanillin.Secondly, adopt simple still distillation, material remains static in still substantially, the static liquid level height, and material evaporation difficulty, the material superheating temperature is big, can produce serious polymerization, decomposition, carbonization phenomenon, reduces the yield of vanillin food grade,1000.000000ine mesh.Secondary simple distillation is heated material repeatedly in former technology, and during underpressure distillation especially for the second time, the content of vanillin food grade,1000.000000ine mesh is very high in the material, and high-temperature heating polymerization decomposing phenomenon is even more serious, causes the vanillin food grade,1000.000000ine mesh yield seriously to reduce.
Along with the raising of Chemicals working depth and the continuous appearance of special-purpose macromole specialty chemicals, the handled high-solidification point of rectifying, the thermo-sensitivity system is more and more.The rectifying of high-solidification point system has high temperature, high vacuum, high-solidification point characteristics.So-called thermo-sensitivity system is exactly that polymerization, decomposition, coking, carbonization phenomenon easily take place under the high-temperature heating situation.For overcoming the service temperature that this phenomenon will reduce rectifying, shorten the heated time of material, avoid material to cross heat-storage.Usually adopt the method for rectification under vacuum, and reduce the tower pressure drop to greatest extent, adopt the reboiler of special shape, eliminate elevation of boiling point phenomenon.High solidifying point material is the difficult problem of distillation operation equally, as deals with improperly not only and can stop up transfer line, and can be at overhead condenser, separates out solid phase in backflow facility and the tower, makes operation be difficult to carry out.These singularity of the rectifying separation of high-solidification point thermo-sensitivity system are brought many difficulties to rectifying.It is very difficult handling these problems with the rectifying device of routine.
Common batch fractionating tower has a very big still usually, and material at first adds in the still during driving, and product is steamed by cat head.For the reboiler of common batch fractionating tower, generally be arranged in the tower still direct heating tower still material.The shortcoming of this structure is the elevation of boiling point that long-term existence fluid column static pressure causes in the tower still, thereby material overstand in hot environment causes the decomposition of heat-sensitive material, polymerization, problems such as carbonization.And along with the carrying out of rectifying, liquid level is more and more lower in the tower still, and the hot face of tower still exposes outside the liquid layer, and the hot face that material is utilized reduces, and is difficult to light constituent is steamed clean, influences product yield.Another shortcoming of this pattern rectifying tower is under high vacuum condition, because the final remaining material viscosity of tower still is very big, occurs membrane type boiling heat transfer or boiling explosion phenomenon easily, and heat-transfer effect is low, and material is overheated bigger, divides the carbonization phenomenon that depolymerizes even more serious.
For continuous rectifying tower,, also can run into the problem same with batch fractionating as the structure of not improving the tower still and the pattern of reboiler.
In order to solve the various shortcoming in the former process for refining, present inventors have invented the highly efficient distilling device that is used for refining crude vanillin, make the sepn process of crude vanillin be reduced to a step distillation operation, a underpressure distillation, toluene crystallization, secondary underpressure distillation and four step of solvent recuperation operation in the former technology have been replaced, avoided in the former sepn process because the overheated polymerization that causes of material, coking, carbonization phenomenon has improved the yield for the treatment of process.
The object of the present invention is to provide a kind of rectifier unit that is used for refining crude vanillin.Another object of the present invention provides a kind of process for refining of vanillin food grade,1000.000000ine mesh, particularly a kind of novel process with special extract rectification device of refining crude vanillin, can directly obtain purity and reach vanillin food grade,1000.000000ine mesh more than 99%, and can effectively overcome the various shortcoming of existing crude vanillin rectification flow.Further purpose of the present invention is to have replaced twice underpressure distillation, toluene solvant crystallization and four operations of solvent recuperation in the former technology with a step rectifying separation operation, the loss of having avoided vanillin food grade,1000.000000ine mesh being heated repeatedly in treating process, oxidation, polymerization, decomposition to cause, toluene crystallization and solvent recuperation operation have been avoided, the investment of reduction equipment, improved yield, reduce energy consumption, material consumption, thereby finished the present invention.
The object of the present invention is achieved like this, a kind of rectifier unit that is used for refining crude vanillin, it is characterized in that this rectifier unit comprises high-efficient spiral-screen column, tower still with cold memory function, tower still recycle pump, the falling film type reboiler, with tower body be the condenser of one, built-in reflux ratio controller and some basins are formed.Rectifying tower adopts overhead condenser and the built-in reflux ratio sparger that directly links to each other with cat head.Gas distributor adopts low pressure drop whirlwind-type gas distributor in the rectifying Tata.Rectifying Tata still is provided with refrigerating unit and has cold memory function.Efficient structured packing is housed in the tower, rectifying tower adopts falling film evaporation formula reboiler, adopt pump circulation falling liquid film reboiler to require to be provided with tower still recycle pump, tower still pump entry and tower still link, circulating-pump outlet and reboiler link, rectifying tower is when operation, material in the tower still flows to reboiler, heating evaporation in reboiler through tower still recycle pump, the gaseous phase materials of evaporation, the packing layer that enters rectifying tower separates, and unevaporated liquid phase material enters the tower still, participates in circulating and evaporating again, rectifying tower adopts decompression operation, and absolute pressure is at 1mmHg～50mmHg in the tower.Reflux ratio 10: 1～1: 10,130～160 ℃ of tower top temperatures, 160～200 ℃ of tower still temperature.This method equipment therefor comprises high-efficient spiral-screen column, overhead condenser and built-in reflux ratio distributor that tower still recycle pump, forced cyclic type falling liquid film reboiler and cat head directly link to each other.Adopt single tower periodical operation also can adopt the multitower operate continuously.The rectifying tower operational condition is tower still absolute pressure 1～20mmHg, reflux ratio 10: 1～1: 10,130 ℃～160 ℃ of tower top temperatures, 160 ℃～200 ℃ of tower still temperature.When adopting periodical operation, middle runnings can be carried out multiple steaming, to improve the vanillin food grade,1000.000000ine mesh yield.The thermo-sensitivity system often has a specific sensitive temperature, surpasses temperature, and the speed of polymerization, decomposition, coking rises rapidly.Therefore the distillation operation of thermo-sensitivity system will be controlled at below the sensitive temperature.Often require the tower still to have very high vacuum tightness in this case.Separate high-solidification point thermo-sensitivity system with common rectifying tower, because column plate or packing layer and column internals resistance are big, the pressure reduction of rectifying tower cat head and tower still is very big, to making the tower still not reach desired vacuum tightness, tower still service temperature is raise.Cause polymerization, decompose, coking phenomenon is difficult to avoid.
Separate high-solidification point thermo-sensitivity system with common rectifying tower, because the zero pour height of material, condenser and backflow distribution circuit are longer, tend to take place line clogging, material is difficult for the difficulty of conveying, simultaneously because tower body, condenser, reflux ratio distributor, outer pipeline internal memory liquid measure are big, shortcomings such as the transition segment length of batch fractionating make the distillation once through yield low.
Singularity for high-solidification point thermo-sensitivity system is brought difficulty to distillation operation, and present inventors adopt the falling film type reboiler, to improve tower still type of heating, prevent that material is overheated; Adopt high efficiency low pressure drop filler, low pressure drop column internals (phegma collector, sparger, supporting plate and pressing plate etc.) and low pressure drop gas distributor, will put in order the tower pressure drop and drop to bottom line, improve tower still vacuum tightness, reduce the distillation operation temperature; Overhead condenser and tower body are designed to one, and adopt built-in reflux ratio distributor, avoid pipeline to connect, avoided line clogging.Solve many difficult problems of high-solidification point thermo-sensitivity system rectifying, thereby finished the present invention.
A kind of rectifier unit that separates the vanillin food grade,1000.000000ine mesh raw product of the present invention is characterized in that adopting the highly efficient distilling device of particular design, and crude vanillin can obtain high purity vanillin food grade,1000.000000ine mesh product through an one-step refining.
Vanillin food grade,1000.000000ine mesh process for refining of the present invention can adopt single tower periodical operation also can adopt the multitower operate continuously, when adopting periodical operation, has very high once through yield, and middle runnings can be carried out multiple steaming, to improve the vanillin food grade,1000.000000ine mesh yield.
Rectifier unit of the present invention adopts the high-efficient spiral-screen column of particular design, and the filler of high separating efficiency, low pressure drop is housed in the tower; Rectifying tower adopts falling film evaporation formula reboiler, adopts pump circulation falling liquid film reboiler to require tower still recycle pump is set, and tower still pump entry and tower still link, and circulating-pump outlet and reboiler link.Rectifying tower is when operation, and the material in the tower still flows to reboiler through tower still recycle pump, heating evaporation in reboiler, and the gaseous phase materials of evaporation, the packing layer that enters rectifying tower separates, and unevaporated liquid phase material enters the tower still, participates in circulating and evaporating again.
In order to reduce the service temperature of rectifying, rectifying tower adopts decompression operation, and absolute pressure is 1mmHg～50mmHg in the tower.Reflux ratio 10: 1～1: 10,130～160 ℃ of tower top temperatures, 160～200 ℃ of tower still temperature.
The rectifying tower that the present invention adopts is a packing tower, and the filler of interior dress high separating efficiency, low pressure drop is preferably regular corrugated wire gauze packing.
Rectifying tower adopts falling film evaporation formula reboiler, preferably adopts forced cyclic type tubulation falling liquid film reboiler.Adopt pump circulation falling liquid film reboiler to require tower still recycle pump is set, tower still pump entry and tower still link, and circulating-pump outlet and reboiler link.Rectifying tower is when operation, and the material in the tower still through tower still recycle pump, flows to reboiler, heating evaporation in reboiler, and the gaseous phase materials of evaporation, the packing layer that enters rectifying tower separates, and unevaporated liquid phase material enters the tower still, participates in circulating and evaporating again.Material forms liquid film on the inwall of the falling liquid film pipe of reboiler, the rate of heat transfer height, and the material superheating temperature is little, and the liquid phase heated time is short.
The present invention can adopt batch distillation process to realize with the technology of rectified purified vanillin food grade,1000.000000ine mesh, also can adopt the continuous rectification process to realize.
Adopt rectifier unit of the present invention, only need a step rectification working process thoroughly to separate vanillin food grade,1000.000000ine mesh and other weight component, directly obtain purity and reach vanillin food grade,1000.000000ine mesh more than 99%, thereby saved the toluene crystallisation process, avoid the loss of vanillin food grade,1000.000000ine mesh and solvent toluene in the toluene crystallisation process, saved single flash simultaneously, reduced the loss that thermopolymerization brought of vanillin food grade,1000.000000ine mesh, reduce energy consumption significantly, improved the economic benefit of factory.
Fig. 1 is the FB(flow block) of former vanillin food grade,1000.000000ine mesh separating technology.
Fig. 2 is the FB(flow block) of vanillin food grade,1000.000000ine mesh separating technology of the present invention.
Fig. 3 is the schematic flow sheet that the present invention adopts batch fractionating.
Fig. 4 is the schematic flow sheet that the present invention adopts continuous rectification.
Fig. 5 is the rectifier unit that the present invention is used to separate crude vanillin.
Describe crude vanillin separator of the present invention in detail below in conjunction with accompanying drawing.
Adopt the flow process of batch fractionating as shown in Figure 3. Thick vanillic aldehyde in the raw material storage tank 1 is added in the tower bottom of rectifying tower 2. In distillation process, the material in the tower reactor 2 is sent into reboiler 4 by tower reactor circulating pump 3, is subjected to thermal evaporation in reboiler, enters rectifying column 5 and separates. The light component that steams condensation in overhead condenser 6 is collected and is entered reflux ratio distributor 7, and reflux ratio distributor is divided into reflux thigh and extraction thigh to condensate liquid, in strand reflux column that refluxes, outside the extraction stock-traders' know-how extraction mouth extraction tower. In operating process, steam front-end volatiles, middle transition cut and vanillic aldehyde cut from cat head successively, be collected in respectively front-end volatiles tank 8, middle transition distillate drum 9 and vanillic aldehyde distillate drum 10. Distillation finishes, and the restructuring that stays in the tower reactor 2 divides tar to discharge outside the tower. Midbarrel is returned in the tower reactor when next operates, and further separates vanillic aldehyde cut wherein.
Adopt the flow process of continuous rectification shown in Fig. 4. Crude product vanillic aldehyde in the head tank 21 adds first rectifying column 23 continuously through feed pump 22, steams the light component ortho vanillin from cat head, is collected in the light component collecting tank 28. Tower reactor circulating pump 24 feeds falling-film reboiler 25, heating evaporation continuously to the material in the tower reactor. The tower reactor circulating pump 24 double discharging pump of first rectifying column 23 and the feed pumps of Second distillation column 210 done. Material-vanillic aldehyde in the tower reactor of first rectifying column and restructuring divide tar to send into continuously Second distillation column. In Second distillation column, the vanillic aldehyde cut steamed from cat head and be collected in the vanillic aldehyde collecting tank 15. Restructuring enters in the tar collecting tank 16 at the bottom of dividing tar by tower at the bottom of the tower.
When batch fractionating operates, at first 50 ℃～80 ℃ material-crude product vanillic aldehyde is added in the tower reactor. Start pumped vacuum systems, set up required vacuum in the tower. The reboiler heating starts the tower reactor circulating pump, the beginning distillation procedure. In the still-process, reflux ratio is controlled at 10: 1～1: 10 range. Cat head steams the ortho vanillin cut successively, midbarrel and vanillic aldehyde cut, and each cut is collected respectively. The vanillic aldehyde cut purity that steams reaches 99%(WT) more than. Distill complete, from tower reactor, emit the restructuring branch-tar. Midbarrel is returned in the tower reactor when next operates, and further reclaims wherein vanillic aldehyde cut.
When continuous rectification operates, two packed tower serial operations that pattern is identical. Model two towers are required vacuum separately, with feed pump material-crude product vanillic aldehyde is added in first tower continuously, steams continuously ortho vanillin from cat head. Vanillic aldehyde and restructuring divide tar to discharge at the bottom of tower continuously, send into after-fractionating tower. Steam the vanillic aldehyde cut from the cat head of second tower, purity reaches 99%(WT) more than. From tower reactor, discharge continuously restructuring branch-tar.
The present invention separates FB(flow block) that vanillic aldehyde semifinished product and former separating technology (Fig. 1) contrast as shown in Figure 2 with device for effectively separating, owing to adopted the highly efficient distilling device, the separative efficiency height, only can thoroughly separate vanillic aldehyde and other weight component through a step rectification working process, obtain purity and reach vanillic aldehyde more than 99%.
Referring to Fig. 5, a kind of rectifier unit for the separation of high-solidification point thermal sensitivity system. This rectifier unit mainly consists of the following components, and the packed tower 32 of high efficiency low pressure drop particular design has the tower reactor 31 of cold memory function, tower reactor circulating pump 38, falling-film reboiler 37, with the condenser 36 that tower body is integrated, built-in reflux ratio controller and some basins form.
High efficiency packing rectifying column among the present invention, in-built efficient separating filler 34 is such as regular wavy metal wire packing. The advantages such as this pattern filler has the separative efficiency height, and the low pressure drop dispersed phase holdup is little can reduce bed stuffing height-namely the reduced height overall of tower greatly. Adopt the low pressure drop filler, can make destilling tower when decompression operation, tower reactor obtains higher vacuum, and the operating temperature of distillation process is reduced.
The reboiler that this rectifier unit adopts is the falling-film evaporating reboiler, is preferably forced circulation falling-film evaporating reboiler. Reboiler is similar to a vertical shell and tube of placing and changes Hot device, material enters heat exchanger from top, material is uniformly distributed in the inwall of heat exchanger-falling film evaporation pipe by filming device, be subjected to thermal evaporation in evaporation tube, used filming device is conventional used various filming devices, such as natural overflow-type, screen cloth film overflow-type, the umbrella formula, spiral etc. Adopt the falling-film evaporating reboiler to make the heat transfer efficiency height, the material heated time is short, does not have the hydrostatic level impact, and the material degree of superheat is little, has avoided the polymerization that causes because material is overheated, the shortcomings such as decomposition.
Rectifying column among the present invention has adopted cyclone gas distributing machine 33, is subjected to the gaseous phase materials of thermal evaporation from reboiler 37, enters in the tower to make gas phase form an eddy flow through a spiral gas distributor, reaches the uniform purpose of gas branch. Spiral gas distributor is made of the helical baffle around the centroclinal placement of tower of some. This cyclone gas distributing machine resistance is little, and distribution of gas is even, can reduce the pressure drop of tower, makes tower reactor keep as far as possible high vacuum, to reach the purpose that reduces tower reactor 31 temperature.
The condenser of the rectifying column among the present invention directly places cat head and adopts built-in reflux ratio controller, the liquid phase material that condenser condenses is got off directly enters cat head liquid phase collector, send into the reflux ratio controller in the tower after the collection, do the distribution that refluxes with extraction, tell reflux thigh and extraction thigh by corresponding reflux ratio, the thigh that refluxes refluxes from the liquid phase distributor that directly enters in the tower, and the extraction thigh is by the extraction of extraction mouth. Condenser 36 is placed on the cat head, reduces SR and has avoided connecting and the shortcomings such as pipeline blockage that cause with pipeline.
Adopt built-in reflux ratio controller 35, avoided material is drawn outside the tower, do the complex equipment of pro rate, pipeline is long, and the shortcomings such as easy obstruction make reflux ratio control simple and direct, easy to operate. The inductance coupling formula reflux in tower that built-in reflux ratio distributor can adopt University Of Tianjin petrochemical technology development centre to manufacture and design compares distributor than distributor or ratio adjusting valve formula reflux in tower.
Adopted the still material pot with cooling infrastructure, material most of the time in distillation process is under the lower temperature conditions, this rectifying to the thermal sensitivity system is very important.
With embodiment implementation method of the present invention is described below, but scope of the present invention is not limited to embodiment.
Separate crude vanillin with batch fractionating tower, rectifying tower tower height 4m, tower diameter 150mm, in adorn self-contained screen waviness packings, bed stuffing height 2m.Tower still recycle pump is given shell and tube falling liquid film reboiler mass transport.In the crude vanillin, contain vanillin food grade,1000.000000ine mesh 78%, ortho vanillin 5%, heavy constituent impurity 17% adds the tower still to the crude vanillin of 50Kg50～80 ℃.Rectifying tower is set up vacuum, keeps tower still absolute pressure 5mmHg.Tower still recycle pump is started in the reboiler heating, begins distillation.Owing to be batch fractionating, rectifying tower is the alternating temperature operation, tower top temperature rises to 155 ℃ gradually by 130 ℃, tower still temperature rises to 190 ℃ gradually by 160 ℃, steam ortho vanillin from cat head successively, middle runnings and contraposition vanillin food grade,1000.000000ine mesh get vanillin food grade,1000.000000ine mesh 30.25Kg, purity 99.61%(WT), once through yield is: 77.26%.
Employing and embodiment 1 identical rectifying tower separates crude vanillin.Add the middle runnings 8.7Kg that crude product vanillin food grade,1000.000000ine mesh 50Kg and last batch operation are collected in the tower still, contain vanillin food grade,1000.000000ine mesh 68% in the middle runnings, obtain vanillin food grade,1000.000000ine mesh 36.25Kg, purity 99.60%(WT), yield is: 92.6%.
Adopt the distillation tower of pattern similarly to Example 1, two tower serial operations separate the vanillin food grade,1000.000000ine mesh raw product with the method for continuous still battery, and two tower packing layer heights are respectively 4M and 2M.The first tower input speed is 25kg per hour.135 ℃ of tower top temperatures, 162 ℃ of tower still temperature, tower still absolute pressure 10mmHg.In first tower, steam ortho vanillin.Cat head discharging 2.5Kg/hr.The tower still material of first tower is directly sent into the second column distillation column distillation.155 ℃ of the second column overhead temperature, 190 ℃ of tower still temperature, tower still absolute pressure 5mmHg.Cat head gets vanillin food grade,1000.000000ine mesh 18.2kg/hr, and purity reaches 99.54%(WT), the tower still is discharged heavy constituent impurity-tar, and yield is: 92.9%.
Claims (7)
1, a kind of rectifier unit that is used for refining crude vanillin, it is characterized in that this rectifier unit adopts the high-efficient spiral-screen column of particular design, tower still with cold memory function, tower still recycle pump, the falling film type reboiler, with tower body be the condenser of one, built-in reflux ratio controller and some basins are formed.
2, rectifier unit according to claim 1 is characterized in that described rectifying tower adopts efficient structured packing.
3, rectifier unit according to claim 1 is characterized in that described rectifying tower adopts overhead condenser and the built-in reflux ratio distributor that directly links to each other with cat head.
4, rectifier unit according to claim 1 is characterized in that described rectifying tower adopts the low pressure drop of particular design, low dispersed phase holdup internals and whirlwind-type gas distributor.
5,, it is characterized in that described rectifying Tata still is provided with refrigerating unit and has cold memory function according to the described rectifier unit of claim 1.
6, rectifier unit according to claim 1 is characterized in that this device can be designed to successive processes, also can be designed to intermittent process.
7, rectifier unit according to claim 1, it is characterized in that in the device for effectively separating rectifying tower, high separating efficiency being housed, the filler of low pressure drop, rectifying tower adopts falling film evaporation formula reboiler, adopt pump circulation falling liquid film reboiler to require to be provided with tower still recycle pump, tower still pump entry and tower still link, circulating-pump outlet and reboiler link, rectifying tower is when operation, and the material in the tower still flows to reboiler through tower still recycle pump, heating evaporation in reboiler, the gaseous phase materials of evaporation, the packing layer that enters rectifying tower separates, and unevaporated liquid phase material enters the tower still, participate in circulating and evaporating again, rectifying tower adopts decompression operation, in the tower absolute pressure at 1mmHg～50mmHg, reflux ratio 10: 1～1: 10,130～160 ℃ of tower top temperatures, 160～200 ℃ of tower still temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95102143A CN1038672C (en) | 1995-03-11 | 1995-03-11 | Rectifying device for refining crude vanillin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95102143A CN1038672C (en) | 1995-03-11 | 1995-03-11 | Rectifying device for refining crude vanillin |
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| CN1109861A true CN1109861A (en) | 1995-10-11 |
| CN1038672C CN1038672C (en) | 1998-06-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95102143A Expired - Fee Related CN1038672C (en) | 1995-03-11 | 1995-03-11 | Rectifying device for refining crude vanillin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101033411B (en) * | 2007-04-19 | 2010-11-24 | 龙岩卓越新能源发展有限公司 | Continuous rectification apparatus for biological diesel oil |
| CN101961562A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Rectification device |
| CN102091432A (en) * | 2010-12-23 | 2011-06-15 | 厦门金达威集团股份有限公司 | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device |
| US9018421B2 (en) | 2008-07-18 | 2015-04-28 | Rhodia Operations | Separation of aromatic aldehydes |
| CN106316815A (en) * | 2016-08-15 | 2017-01-11 | 津鼎（上海）化工技术服务中心 | Preparation method and implementation device thereof for refined vanillin |
| CN108299238A (en) * | 2018-04-03 | 2018-07-20 | 烟台国邦化工机械科技有限公司 | A kind of cyanoacetate or malonate recovery process method and device |
| CN111265902A (en) * | 2020-03-09 | 2020-06-12 | 内蒙古兰格生物科技有限公司 | Continuous rectification device |
| CN111957062A (en) * | 2020-09-11 | 2020-11-20 | 赵汇川 | Reduced pressure distillation device and process for continuous desalting of crude glycerol |
| CN114146439A (en) * | 2021-12-10 | 2022-03-08 | 北京道思克矿山装备技术有限公司 | Double-falling-film evaporation rectifying tower system and rectifying method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6040991A (en) * | 1983-08-15 | 1985-03-04 | 株式会社日立製作所 | Fuel support structure |
| DE3533562A1 (en) * | 1985-09-20 | 1987-04-02 | Krupp Gmbh | METHOD FOR OBTAINING VANILLIN |
-
1995
- 1995-03-11 CN CN95102143A patent/CN1038672C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033411B (en) * | 2007-04-19 | 2010-11-24 | 龙岩卓越新能源发展有限公司 | Continuous rectification apparatus for biological diesel oil |
| US9018421B2 (en) | 2008-07-18 | 2015-04-28 | Rhodia Operations | Separation of aromatic aldehydes |
| CN101961562A (en) * | 2010-10-19 | 2011-02-02 | 常州吉恩化工有限公司 | Rectification device |
| CN101961562B (en) * | 2010-10-19 | 2012-09-26 | 常州吉恩化工有限公司 | Rectification device |
| CN102091432A (en) * | 2010-12-23 | 2011-06-15 | 厦门金达威集团股份有限公司 | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device |
| CN102091432B (en) * | 2010-12-23 | 2013-01-09 | 厦门金达威集团股份有限公司 | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device |
| CN106316815A (en) * | 2016-08-15 | 2017-01-11 | 津鼎（上海）化工技术服务中心 | Preparation method and implementation device thereof for refined vanillin |
| CN108299238A (en) * | 2018-04-03 | 2018-07-20 | 烟台国邦化工机械科技有限公司 | A kind of cyanoacetate or malonate recovery process method and device |
| CN108299238B (en) * | 2018-04-03 | 2024-01-19 | 烟台国邦化工机械科技有限公司 | Process and device for recycling cyanoacetate or malonate |
| CN111265902A (en) * | 2020-03-09 | 2020-06-12 | 内蒙古兰格生物科技有限公司 | Continuous rectification device |
| CN111957062A (en) * | 2020-09-11 | 2020-11-20 | 赵汇川 | Reduced pressure distillation device and process for continuous desalting of crude glycerol |
| CN114146439A (en) * | 2021-12-10 | 2022-03-08 | 北京道思克矿山装备技术有限公司 | Double-falling-film evaporation rectifying tower system and rectifying method thereof |
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