CN101891672B - Separation and purification method and device for extracting and purifying piperidinol product from piperidone hydrogenation reaction solution - Google Patents
Separation and purification method and device for extracting and purifying piperidinol product from piperidone hydrogenation reaction solution Download PDFInfo
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- CN101891672B CN101891672B CN2010102198201A CN201010219820A CN101891672B CN 101891672 B CN101891672 B CN 101891672B CN 2010102198201 A CN2010102198201 A CN 2010102198201A CN 201010219820 A CN201010219820 A CN 201010219820A CN 101891672 B CN101891672 B CN 101891672B
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Abstract
The invention discloses a separation and purification method and a device for extracting and purifying a piperidinol product from piperidone hydrogenation reaction solution, and the method comprises the following steps: (a) leading piperidinol crude product raw material solution into a feed inlet of a piperidone recovery distillation column, discharging light components of piperidone, acetonine and the like from the top of the piperidone recovery distillation column, then condensing by a recovery condenser, leading part of the light components to return and simultaneously extracting part of the light components as a piperidone product; and (b) sending the materials extracted from the bottom part of the piperidone recovery distillation column into the feed inlet of a piperidinol rectification column, extracting gas phase piperidinol from the top of the piperidinol rectification column, condensing the gas phase piperidinol by the condenser, then leading one part to return, simultaneously extracting the other part as a product, heating stillage residue part discharged from the bottom of the piperidinol rectification column by a reboiler at the bottom of the piperidinol rectification column, then forming the gas phase, returning into the column and simultaneously discharging one part as waste liquid. The adoption of the method can obtain the high-purity piperidinol product (above 99.5% by weight) at one time and recover the piperidone product.
Description
Technical field
The present invention relates to a kind of separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution, also relate to a kind of separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution.
Background technology
Traditional piperidines alcohol (2,2,6 as shown in Figure 1; 6-tetramethyl--4-piperidines alcohol) production technique be earlier with acetone as basic material, after reacting, obtain piperidone, again with piperidone (2; 2,6,6-tetramethyl--4-piperidone) obtains piperidines alcohol bullion behind the hydrogenation; Be component mixing solutionss such as a kind of piperidines alcohol, piperidone and acetonines involved in the present invention; Through (this moment, piperidines alcohol quality percentage composition about about 90%) after simply removing alcohol, carry out crystallization first time, the piperidines that obtains 95%-97% is pure.Then, could finally obtain the product more than 99.5% through secondary crystal again.Because shortcomings such as the crystalline element operating process are long, equipment is many, loss of material is big, labour intensity is big, the piperidinol product that causes two times of crystallization post crystallization mother liquor to take away is more, must reduce the single loop yield of product, and the acetone consumption of ton product is bigger.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the separating and purifying method of the extracting and purifying piperidinol product from piperidone hydrogenation reaction solution that a kind of raw materials consumption is few, product purity is high and blowdown flow rate is little is provided.
Another object of the present invention is to provide a kind of separation purifying plant with extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of energy-efficient, safety and stability advantage.
The separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of the present invention, it may further comprise the steps:
(a) piperidines alcohol bullion liquid stock is fed piperidone recovery distillation tower middle part opening for feed, light constituents such as piperidone and acetonines are discharged from the cat head of said piperidone recovery distillation tower after reclaim the backflow of condenser condenses rear section simultaneously partly as the extraction of piperidone product; The cat head working pressure that described piperidone reclaims distillation tower is-0.090～0.080MPa, and the pressure reduction at the bottom of cat head and the tower is 1～3kPa;
(b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.090～-0.080MPa, the pressure reduction at the bottom of cat head and the tower is 2～3kPa.
The separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of the present invention; It comprises that piperidone reclaims distillation tower and piperidines alcohol rectifying tower; The cat head that reclaims distillation tower and piperidines alcohol rectifying tower at described piperidone is connected with condensation and is connected with reboiler respectively with reflux and in the tower bottom of piperidone recovery distillation tower and the pure rectifying tower of piperidines; The middle part of reclaiming distillation tower and piperidines alcohol rectifying tower tower body at piperidone has opening for feed; Discharge port links to each other through the opening for feed of pipeline with described piperidines alcohol rectifying tower at the bottom of the tower of described piperidone recovery distillation tower, at the bottom of the tower of described piperidines alcohol rectifying tower, is connected with the waste liquid pipeline.
Adopt the beneficial effect of the inventive method and device to be:
1) is improved to the continuous reduced pressure distillation technique of double tower of the present invention by traditional Crystallization Separation purifying technique, once can obtains highly purified piperidinol product (mass percent is more than 99.5%), and reclaim the piperidone product;
2) shorten separation process, improved separation efficiency; Reduce labor strength, reduced the discharging of pollutent.
3) adopt the method for design of " evaporation-condensation " formula condensing surface, practiced thrift the consumption of water coolant, reclaimed the distillation waste heat, reduced producing.
4) adopt low pressure drop structured packing and forced circulating reboiler, reduced distillation still residue temperature-sensitive coking amount, improved product yield.
Description of drawings
Fig. 1 is traditional crystallization separation process sketch;
Fig. 2 is the general flow chart of the separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of the present invention;
Fig. 3 is that piperidines alcohol rectifying tower cat head adopts " evaporation-condensation " formula structure of condenser synoptic diagram in the inventive method.
Embodiment
Below in conjunction with concrete embodiment, and, the present invention is done further explanation with reference to accompanying drawing:
The separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of the present invention as shown in Figure 2; It may further comprise the steps: (a) piperidines alcohol bullion liquid stock is heated to back feeding piperidone recovery distillation tower 1 middle part opening for feed about 70 ℃ usually, light constituents such as piperidone and acetonines are discharged after reclaim condensing surface 3 condensation rear sections backflow while part as the extraction of piperidone product from the cat head that said piperidone reclaims distillation tower; The cat head working pressure that described piperidone reclaims distillation tower is-0.090～0.080MPa (absolute pressure), and the pressure reduction at the bottom of cat head and the tower is 1～3kPa; (b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower 4; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.090～-0.080MPa (absolute pressure), the pressure reduction at the bottom of cat head and the tower is 2～3kPa.
The recovery condensing surface of the distillation tower of piperidone recovery in the methods of the invention cat head is to link to each other with cat head through the gas phase pipeline; The liquid material that the device condensation that is condensed is got off gets into return tank; A part is as the essential withdrawing fluid of distillation tower; This liquid gets in the trim the top of column sparger through reflux pump, and the material that exports out from reflux pump is except that a backflow part, and a part gets into piperidone product jar in addition.From the liquid phase material major part of the liquid extraction mouth extraction of the bottom of piperidone regenerating column is piperidines alcohol; The higher heavy constituent impurity of ratio piperidines alcohol boiling point that has only few part, this strand material are transported to the charging of the intermediate feed mouth of piperidines alcohol rectifying tower as piperidines alcohol rectifying tower.
The tower bottom reboiler of preferred described piperidines alcohol rectifying tower adopts pump circulation, can accelerate the flow velocity of material like this, thereby avoid the bottoms material to solidify, and stops up the reboiler heat transfer tube.
The piperidone regenerating column reclaims condensing surface can select traditional fixed tube sheet heat exchanger for use, and refrigerant gets final product with one recirculated cooling water, can not be lower than 45 ℃ but will control the temperature that piperidone is condensed, because the piperidone zero pour is 39 ℃.When being lower than this temperature, piperidone will be solidified, and stop up interchanger, and parking causes the accident when serious.The trim the top of column of the piperidines alcohol rectifying tower in preferably described (b) step adopts internal reflux and overhead condenser to adopt soft water as refrigerant.Piperidines alcohol rectifying tower overhead condenser is directly designed at cat head; Link together by shell flange with tower body; Gaseous phase materials can get into condensing surface heat transfer tube interior passageway more fastly like this; The liquid material that the device condensation that is condensed is got off is directly got back in the scoop of topmost, condensing surface heat transfer tube bottom of this tower, and a part is as the essential withdrawing fluid of distillation tower, and this liquid gets in the overhead liquid distribution of reflux device through fluid conduits; The liquid of part is drawn outside the tower near the local extraction pipe of scoop from cat head in addition, gets into the piperidinol product jar.
Piperidines alcohol rectifying tower cat head " soft water evaporation-condensation formula " condensing surface is used in piperidines alcohol cat head, and this condensing surface preferably adopts 40-50 ℃ of soft water as initial refrigerant, gets into the shell side of this condensing surface.When soft water after heat absorption vaporization under the certain pressure, be discharged from the condensing surface shell side through the vapour line that is welded on shell side top, this vapor pressure is at 0.3-0.4MPa, can guarantee like this piperidines alcohol rectifying tower top working pressure-0.090～-0.080MPa.Why be because it is less scaling, guarantee that the heat transfer coefficient of condensing surface is higher with soft water.
The separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution of the present invention; It comprises that piperidone reclaims distillation tower 1 and piperidines alcohol rectifying tower 4; The cat head that reclaims distillation tower and piperidines alcohol rectifying tower at described piperidone is connected with reflux and is connected with reboiler 2,5 respectively in the tower bottom of piperidone recovery distillation tower and piperidines alcohol rectifying tower; The middle part of reclaiming distillation tower and piperidines alcohol rectifying tower tower body at piperidone has opening for feed; Discharge port links to each other through the opening for feed of pipeline with described piperidines alcohol rectifying tower at the bottom of the tower of described piperidone recovery distillation tower, at the bottom of the tower of described piperidines alcohol rectifying tower, is connected with the waste liquid pipeline.
The reflux that described piperidone reclaims distillation tower is an external reflux device.
The condensation and the reflux of preferred described piperidines alcohol rectifying tower are interior condensation and reflux 6.Condensation and reflux can comprise housing in described; Vertically be provided with a plurality of heat transfer tube 6-1 and on this place's housing, have water-in 6-3 and vapour outlet 6-2 at described housing internal upper part; In the housing of described heat transfer tube bottom, traverse baffle is housed; Scoop links to each other with described inner walls along the circumferential direction setting of inner walls and the diapire of scoop; Training wall near the traverse baffle of inner walls setting is positioned at the top at described scoop top so that the water conservancy diversion fluid power enough flows into described scoop; Be positioned on the housing of described scoop position and have material extraction mouth 6-4; The bottom is provided with liquid return sparger 6-6 in described housing, and the bottom of described scoop is connected with described liquid return sparger through thrust-augmenting nozzle 6-5, and described housing bottom is connected through shell flange with the cat head of piperidines alcohol rectifying tower 4.
The tower bottom reboiler of preferred described piperidines alcohol rectifying tower is a forced circulating reboiler.
The tower body that preferably reclaims distillation tower and the pure rectifying tower of piperidines at piperidone is outside equipped with insulation jacket or heat-insulating coil pipe, like this to device open, proper when stopping.
Piperidines alcohol bullion liquid stock is heated to 70 ℃ feeds piperidone recovery distillation tower 1 middle part opening for feed, light constituents such as piperidone and acetonines reclaim the cat head discharge of distillation tower from said piperidone and reflux the while part as the extraction of piperidone product after reclaim condensing surface 3 condensation rear sections; The cat head working pressure that described piperidone reclaims distillation tower is-0.090MPa (absolute pressure, down together) that the pressure reduction at the bottom of cat head and the tower is 2kPa; (b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower 4; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.085MPa (absolute pressure, down together) that the pressure reduction at the bottom of cat head and the tower is 2.5kPa.The tower bottom reboiler of described piperidines alcohol rectifying tower adopts pump circulation.
Through detecting: piperidinol product quality percent purity is more than 99.5%, and reclaims the piperidone product.
Piperidines alcohol bullion liquid stock is heated to 72 ℃ feeds piperidone recovery distillation tower 1 middle part opening for feed, light constituents such as piperidone and acetonines reclaim the cat head discharge of distillation tower from said piperidone and reflux the while part as the extraction of piperidone product after reclaim condensing surface 3 condensation rear sections; The cat head working pressure that described piperidone reclaims distillation tower is 0.01MPa (absolute pressure), and the pressure reduction at the bottom of cat head and the tower is 1kPa; (b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower 4; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.080MPa that the pressure reduction at the bottom of cat head and the tower is 3kPa.The tower bottom reboiler of described piperidines alcohol rectifying tower adopts pump circulation.Piperidines alcohol rectifying tower cat head adopts " soft water evaporation-condensation formula " condensing surface, and condensing surface adopts 45 ℃ of soft water as initial refrigerant, gets into the shell side of this condensing surface.When soft water after heat absorption vaporization under the certain pressure, through being discharged from the condensing surface shell side with the vapour line that is welded on shell side top, this vapor pressure is at 0.4MPa.
Through detecting: piperidinol product quality percent purity is more than 99.5%, and reclaims piperidone product, byproduct steam 150kg/hr.
Piperidines alcohol bullion liquid stock is heated to 68 ℃ feeds piperidone recovery distillation tower 1 middle part opening for feed, light constituents such as piperidone and acetonines reclaim the cat head discharge of distillation tower from said piperidone and reflux the while part as the extraction of piperidone product after reclaim condensing surface 3 condensation rear sections; The cat head working pressure that described piperidone reclaims distillation tower is 0.040MPa (absolute pressure), and the pressure reduction at the bottom of cat head and the tower is 3kPa; (b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower 4; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.090MPa that the pressure reduction at the bottom of cat head and the tower is 2kPa.The tower bottom reboiler of described piperidines alcohol rectifying tower adopts pump circulation.Piperidines alcohol rectifying tower cat head adopts " soft water evaporation-condensation formula " condensing surface, and condensing surface adopts 50 ℃ of soft water as initial refrigerant, gets into the shell side of this condensing surface.When soft water after heat absorption vaporization under the certain pressure, through being discharged from the condensing surface shell side with the vapour line that is welded on shell side top, this vapor pressure is at 0.3MPa.
Through detecting: piperidinol product quality percent purity is more than 99.5%, and reclaims piperidone product, byproduct steam 150kg/hr.
Piperidines alcohol bullion liquid stock is heated to 70 ℃ feeds piperidone recovery distillation tower 1 middle part opening for feed, light constituents such as piperidone and acetonines reclaim the cat head discharge of distillation tower from said piperidone and reflux the while part as the extraction of piperidone product after reclaim condensing surface 3 condensation rear sections; The cat head working pressure that described piperidone reclaims distillation tower is 0.080MPa (absolute pressure), and the pressure reduction at the bottom of cat head and the tower is 1.5kPa; (b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower 4; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.092MPa that the pressure reduction at the bottom of cat head and the tower is 2kPa.The tower bottom reboiler of described piperidines alcohol rectifying tower adopts pump circulation.Piperidines alcohol rectifying tower cat head adopts " soft water evaporation-condensation formula " condensing surface, and condensing surface adopts 40 ℃ of soft water as initial refrigerant, gets into the shell side of this condensing surface.When soft water after heat absorption vaporization under the certain pressure, through being discharged from the condensing surface shell side with the vapour line that is welded on shell side top, this vapor pressure is at 0.35MPa.
Through detecting: piperidinol product quality percent purity is more than 99.5%, and reclaims piperidone product, byproduct steam 150kg/hr.
Claims (7)
1. the separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution is characterized in that it may further comprise the steps:
(a) piperidines alcohol bullion liquid stock is fed piperidone and reclaim distillation tower middle part opening for feed, piperidone and acetonines light constituent are discharged through reclaiming the condenser condenses rear section from the cat head of said piperidone recovery distillation tower and are refluxed the while part as the extraction of piperidone product; The cat head working pressure that described piperidone reclaims distillation tower is-0.090～0.080MPa, and the pressure reduction at the bottom of cat head and the tower is 1～3kPa;
(b) material that reclaims distillation tower bottom extraction from said piperidone is sent into the middle part opening for feed of piperidines alcohol rectifying tower; At described piperidines alcohol rectifying tower cat head extraction gas phase piperidines alcohol; Gas phase piperidines alcohol refluxes while another part as the product extraction through the condenser condenses rear section; The tower bottom reboiler heating back of the pure rectifying tower of still remnants of defeated troops lease making piperidines of at the bottom of described piperidines alcohol rectifying Tata, discharging forms gas phase and returns in the tower simultaneously partly as discharging of waste liquid; Described piperidines alcohol rectifying tower top working pressure is-0.090～-0.080Mpa, the pressure reduction at the bottom of cat head and the tower is 2～3kPa.
2. the separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution according to claim 1 is characterized in that: the tower bottom reboiler employing pump circulation of described piperidines alcohol rectifying tower.
3. the separating and purifying method of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution according to claim 1 is characterized in that: the trim the top of column of the piperidines alcohol rectifying tower in described (b) step adopts internal reflux and overhead condenser to adopt soft water as refrigerant.
4. the separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution; It is characterized in that: it comprises that piperidone reclaims distillation tower and piperidines alcohol rectifying tower; The cat head that reclaims distillation tower and piperidines alcohol rectifying tower at described piperidone is connected with condensation separately and is connected with reboiler respectively with reflux and in the tower bottom of piperidone recovery distillation tower and the pure rectifying tower of piperidines; The middle part of reclaiming distillation tower and piperidines alcohol rectifying tower tower body at piperidone has opening for feed; Discharge port links to each other through the opening for feed of pipeline with described piperidines alcohol rectifying tower at the bottom of the tower of described piperidone recovery distillation tower, at the bottom of the tower of described piperidines alcohol rectifying tower, is connected with the waste liquid pipeline.
5. the separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution according to claim 4; It is characterized in that: the reflux that described piperidone reclaims distillation tower is an external reflux device, and the condensation and the reflux of described piperidines alcohol rectifying tower are interior condensation and reflux.
6. the separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution according to claim 4; It is characterized in that: described condensation and reflux comprise housing; Vertically be provided with a plurality of heat transfer tubes and on housing, have water-in and vapour outlet at described housing internal upper part; In the housing of described heat transfer tube bottom, traverse baffle is housed; Scoop links to each other with described inner walls along the circumferential direction setting of inner walls and the diapire of scoop; Training wall near the traverse baffle of inner walls setting is positioned at the top at described scoop top so that the water conservancy diversion fluid power enough flows into described scoop; Be positioned at and have material extraction mouth on the housing of described scoop position and be provided with the liquid return sparger in described housing bottom, the bottom of described scoop is connected with described liquid distributor through thrust-augmenting nozzle, and described housing bottom is connected through shell flange with the cat head of piperidines alcohol rectifying tower.
7. the separation purifying plant of extracting and purifying piperidinol product from piperidone hydrogenation reaction solution according to claim 4 is characterized in that: the tower bottom reboiler of described piperidines alcohol rectifying tower is a forced circulating reboiler.
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| CN101906042B (en) * | 2010-06-07 | 2013-11-13 | 浙江禾田化工有限公司 | Separation and purification method and device of alpha-o-methyl phenyl-beta-methoxyl methyl acrylate |
| CN102675187B (en) * | 2011-08-29 | 2014-01-08 | 天津大学 | Refining and continuous production method and device for pipradrol capable of continuously recycling ethanol |
| CN102321013B (en) * | 2011-09-06 | 2013-06-05 | 天津大学 | Piperidone continuous refining production method and device capable of continuously recovering acetone |
| CN103215066B (en) * | 2012-12-12 | 2015-03-25 | 滁州市润达溶剂有限公司 | Distillation separation device and method for liquid hydrocarbon mixture |
| CN108218026B (en) * | 2017-12-08 | 2019-03-05 | 杭州九清科技有限公司 | A method of processing waste water containing piperidine alcohols simultaneously recycles piperidine alcohols |
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