CN101961562B - Rectification device - Google Patents
Rectification device Download PDFInfo
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- CN101961562B CN101961562B CN201010510541A CN201010510541A CN101961562B CN 101961562 B CN101961562 B CN 101961562B CN 201010510541 A CN201010510541 A CN 201010510541A CN 201010510541 A CN201010510541 A CN 201010510541A CN 101961562 B CN101961562 B CN 101961562B
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Abstract
The invention belongs to chemical equipment, in particular to rectification equipment which is used for recovering butyl dicarbonate in crystallized mother liquor. The rectification device comprises a column kettle, a circulating pump, a falling film type reboiler, a pylon, a condenser and a receiving tank. The invention has the advantages of high recovery rate and high product purity of butyl dicarbonate, is especially suitable for recovering butyl dicarbonate in the crystallized mother liquor, improves work efficiency and lowers production cost.
Description
Technical field
The invention belongs to chemical industry equipment, relate to a kind of distillation equipment specifically, be used for reclaiming the rectifier unit of the di-tert-butyl dicarbonate of crystalline mother solution.
Background technology
In the prior art, still contain the di-tert-butyl dicarbonate product about 30% in the mother liquor of the explained hereafter of employing crystallization purifying di-tert-butyl dicarbonate, all the other are solvent and the low impurity dimethyl dicarbonate butyl ester that boils; Existing technology adopts long-time-20 ℃ of low temperature crystallizations to reclaim product; Can only reclaim the product of 5% left and right sides content 95%, reclaim product purity also further exquisiteness processing not up to standard, and the prior art energy consumption be high; Man-hour is long, and operational sequence is loaded down with trivial details.
Summary of the invention
The objective of the invention is to provides a kind of rectifier unit to reclaiming product purity shortcoming not up to standard in the above-mentioned technology, has rate of recovery height, and the advantage of good product purity is applicable to the di-tert-butyl dicarbonate that reclaims in the crystalline mother solution.
The technical scheme that realizes the object of the invention is following:
Rectifier unit, it comprises tower still, circulating pump, falling film type reboiler, king-post, condenser and receiving slit; The tower still is provided with charging aperture and thermometer; Falling film type reboiler one end is located on the tower still top, and the other end is connected with tower still bottom through circulating pump, is provided with heating mechanism in the falling film type reboiler, and this heating mechanism comprises steam inlet and steam (vapor) outlet; King-post is located on the tower still, and the king-post top is provided with gas phase interface tube, thermometer and liquid distributor, and this gas phase interface tube links to each other with condenser; Condenser is provided with gas phase inlet, drain, cooling water inlet, coolant outlet and condensate outlet, and the gas phase inlet is connected with the gas phase interface tube, and condensate outlet is connected with liquid distributor; Comprise on the receiving slit feed liquid inlet, drain with and the drain hole of bottom, the feed liquid inlet also is connected with condensate outlet.
Adopted such scheme; The tower still is used to hold the mother liquor raw material of the explained hereafter of crystallization purifying di-tert-butyl dicarbonate, and the tower still is a cake formula tower still, and cake formula tower still has bigger disengagement area and thin liquid layer; Chuck is used to adjust the temperature of feed liquid in the tower still; Circulating pump is used for the raw material of tower still is sent into the back gasification of heating in the falling film type reboiler, and the raw material after the gasification gets in the king-post and gets into condensation in the condenser by king-post, and condenser is the reflux condenser of shell and tube; There is not the raw material of gasification to pass back in the tower still; Continuation is sent in the falling film type reboiler by circulating pump, and the liquid material part that receives condensation in the condenser is back in the king-post through phegma inlet and liquid distributor, and another part liquid flows into receiving slit.
Described falling film type reboiler is located on the tower still through the concentric reducer connector, and falling film type reboiler top is provided with feed liquid inlet, and the falling film type reboiler is provided with plate hole formula distributor in it, and this feed liquid inlet links to each other with described outlet of circulating pump.
Described tower still is provided with chuck outward, comprises the cooling water inlet and the coolant outlet of the cooling water that is used to circulate on this chuck, and tower still bottom also is provided with the outlet of still liquid, and this still liquid outlet links to each other with said inlet of circulating pump.
Described king-post is divided into two joints, and king-post is provided with the phegma inlet, and described condensate liquid inlet is connected with liquid distributor through this phegma inlet, also is provided with ceramic ripple packing in the king-post.
The rate of recovery that the invention has the advantages that di-tert-butyl dicarbonate is high, and the advantage of good product purity is particularly useful for reclaiming the di-tert-butyl dicarbonate in the crystalline mother solution, has improved operating efficiency, has reduced production cost.
Description of drawings
Fig. 1 is a structural representation of the present invention.
The specific embodiment
As shown in Figure 1, rectifier unit, it comprises tower still 1-4, circulating pump 4, falling film type reboiler 5, king-post 1, condenser 2 and receiving slit 3; Tower still 1-4 is provided with charging aperture 1-5 and thermometer T1; Falling film type reboiler 5 one ends are located on the tower still top, and the other end is connected with tower still bottom through circulating pump 4, is provided with heating mechanism in the falling film type reboiler 5, and this heating mechanism comprises steam inlet 5-3a and steam (vapor) outlet 5-3b; King-post 1 is located on the tower still 1-4, and king-post 1 top is provided with gas phase interface tube 1-1, thermometer T2 and liquid distributor 1-2, and this gas phase interface tube 1-1 links to each other with condenser 2; Condenser 2 is provided with gas phase inlet 2-1, drain 2-2, cooling water inlet 2-4, coolant outlet 2-3 and condensate outlet 2-5, and gas phase inlet 2-1 is connected with gas phase interface tube 1-1, and condensate outlet 2-5 is connected with liquid distributor 1-2; Comprise on the receiving slit 3 feed liquid inlet 3-1, drain 3-2 with and the drain hole 3-3 of bottom, feed liquid inlet 3-1 also is connected with condensate outlet 2-5.
The tower still is used to hold the mother liquor raw material of the explained hereafter of crystallization purifying di-tert-butyl dicarbonate, and the tower still is a cake formula tower still, and cake formula tower still has bigger disengagement area and thin liquid layer; Chuck is used to adjust the temperature of feed liquid in the tower still, and circulating pump is used for the raw material of tower still is sent into the back gasification of heating in the falling film type reboiler, and the raw material after the gasification gets in the king-post and gets into condensation in the condenser by king-post; Condenser is the reflux condenser of the horizontal shell and tube that prevents, walks material in the condenser hypostracum, walks cooling fluid in the pipe layer; Drain is arranged at shell top, is used to supply emptying or vacuumizing, and condensate liquid can pass back into tower also can cause receiving slit; Receiving slit is vertical receiving slit jar; Do not have the raw material of gasification to pass back in the tower still, continue to be sent in the falling film type reboiler by circulating pump, the liquid material part that receives condensation in the condenser is back in the king-post through phegma inlet and liquid distributor; Another part liquid flows into receiving slit; Wherein heating mechanism is a shell and tube reboiler shell Steam Heating mechanism, and steam circulates through steam inlet 5-3a and steam (vapor) outlet 5-3b, and drain 2-2 and drain 3-2 can supply emptying or vacuumizing; Wherein thermometer T1 is used for the temperature in the monitoring tower still 1-4, and thermometer T2 is used for the temperature of monitoring tower capital end.
Wherein, Falling film type reboiler 5 is located on the tower still 1-4 through extra heavy pipe concentric reducer connector 5-4; And falling film type reboiler 5 tops are provided with feed liquid inlet 5-1, and falling film type reboiler 5 is provided with plate hole formula distributor 5-2 in it, and this feed liquid inlet 5-1 links to each other with the outlet 4-2 of described circulating pump 4; Cellular type distributor 5-2 is double-layer porous board-like liquid distributor, and the board-like liquid distributor of this perforated is used for the equally distributed entering falling film type reboiler top of raw material liq.
Wherein, Tower still 1-4 is provided with chuck 1-6 outward; Chuck 1-6 can regulate the temperature of raw material liq in the tower still; The cooling water inlet 1-7a and the coolant outlet 1-7b that comprise the cooling water that is used to circulate on this chuck 1-6, tower still 1-4 bottom also is provided with still liquid outlet 1-8, and this still liquid outlet 1-8 links to each other with the import 4-1 of said circulating pump 4.
Wherein, king-post 1 is divided into two joints, is respectively king-post 1-3a and king-post 1-3b, and king-post 1-3a is provided with phegma inlet 12a, and described condensate liquid inlet 2-5 is connected 1-2 through this phegma inlet 1-2a with liquid distributor, also is provided with ceramic ripple packing in the king-post 1.
Crystalline mother solution is got among the tower still 1-4 by tower still 1-4 charging aperture 1-5; Still liquid outlet 1-8 by tower still bottom gets into still liquid circulating pump 4 through inlet of circulating pump 4-1 then; Get into falling liquid film reboiler charging aperture 5-1 by its outlet 4-2, get in the falling film type reboiler 5 through plate hole formula distributor 5-2 distributed uniform spray.Steam gets into heating by steam inlet 5-3a; The condensed water of steam is discharged by steam (vapor) outlet 5-3b; The still liquid of heating vaporization is got among the tower still 1-4 by concentric reducer connector 5-4; Gas after the gasification is risen by king-post 1-3a, king-post 1-3b, does not have the liquid of gasification then to get into repetitive cycling heating and gasifying in the tower still.Uprising gas is got into by cat head gas phase interface tube 1-1 to the liquid distributor 1-2 and is drawn by bottom condensate outlet 2-5 after being condensed into liquid in the gas phase inlet 2-1 condenser 2 of condenser; Partially liq returns liquid distributor 1-2; Flow to tower still 1-4 along king-post 1-3a, king-post 1-3b then; Another part is then introduced receiving slit 3, and 3-1 inserts by the feed liquid inlet.The cooling water of condenser 2 is introduced the back by cooling water inlet 2-4 and is flowed out by coolant outlet 2-3, is used to provide cold, and the solvent that steams, low-boiling-point substance, di-tert-butyl dicarbonate are discharged by receiving slit bottom discharging opening 3-3 respectively.Through regulating tower top temperature T2; Tower still temperature T 1 and tower still cooling water flow; Tower still cooling water is flowed into by cooling water inlet 1-7a, and coolant outlet 1-7b flows out, and regulates vacuum by drain 2-2 and drain 3-2 simultaneously; Can make di-tert-butyl dicarbonate rate of recovery 85-90%, product purity is more than 99%.
The present invention is mainly used in the di-tert-butyl dicarbonate in the mother liquor raw material of the explained hereafter that reclaims the crystallization purifying di-tert-butyl dicarbonate, can reclaim other compositions in other industrial chemicals, and is effective, and can realize Controllable Temperature, adjustable-speed.
Claims (4)
1. rectifier unit, it is characterized in that: it comprises cake formula tower still, circulating pump, falling film type reboiler, king-post, condenser and receiving slit;
Cake formula tower still is provided with charging aperture and thermometer;
Falling film type reboiler one end is located on the cake formula tower still top, and the other end is connected with cake formula tower still bottom through circulating pump, is provided with heating mechanism in the falling film type reboiler, and this heating mechanism comprises steam inlet and steam (vapor) outlet;
King-post is located on the cake formula tower still, and the king-post top is provided with gas phase interface tube, thermometer and liquid distributor, and this gas phase interface tube links to each other with condenser;
Condenser is provided with gas phase inlet, drain, cooling water inlet, coolant outlet and condensate outlet, and the gas phase inlet is connected with the gas phase interface tube, and condensate outlet is connected with liquid distributor;
Comprise on the receiving slit feed liquid inlet, drain with and the drain hole of bottom, the feed liquid inlet also is connected with condensate outlet.
2. rectifier unit according to claim 1; It is characterized in that: described falling film type reboiler is located on the cake formula tower still through the concentric reducer connector; And falling film type reboiler top is provided with the feed liquid inlet; The falling film type reboiler is provided with plate hole formula distributor in it, and this feed liquid inlet links to each other with described outlet of circulating pump.
3. rectifier unit according to claim 1; It is characterized in that: described cake formula tower still is provided with chuck outward; The cooling water inlet and the coolant outlet that comprise the cooling water that is used to circulate on this chuck; Cake formula tower still still bottom also is provided with the outlet of still liquid, and this still liquid outlet links to each other with said inlet of circulating pump.
4. rectifier unit according to claim 1 is characterized in that: described king-post is divided into two joints, and king-post is provided with the phegma inlet, and described condensate liquid inlet is connected with liquid distributor through this phegma inlet, also is provided with ceramic ripple packing in the king-post.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010510541A CN101961562B (en) | 2010-10-19 | 2010-10-19 | Rectification device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010510541A CN101961562B (en) | 2010-10-19 | 2010-10-19 | Rectification device |
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| CN101961562A CN101961562A (en) | 2011-02-02 |
| CN101961562B true CN101961562B (en) | 2012-09-26 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102309866A (en) * | 2011-09-08 | 2012-01-11 | 中国石油天然气集团公司 | Treating column of cyclic 1, 3-propanediol in continuous production process of poly (trimethylene terephthalate) |
| CN104941228A (en) * | 2014-03-30 | 2015-09-30 | 天津东大化工集团有限公司 | Falling-film evaporator for benzyl benzoate production by using purification method and using method of falling-film evaporator |
| CN105502788A (en) * | 2015-12-31 | 2016-04-20 | 遵义鑫湘生物科技有限公司 | Gallate wastewater disposal system |
| CN108484395A (en) * | 2018-05-02 | 2018-09-04 | 宜兴市恒兴精细化工有限公司 | A kind of device of continuity method synthesis isobutyl isobutyrate |
| CN111001177B (en) * | 2019-12-17 | 2023-05-30 | 安徽昊源化工集团有限公司 | Device for preventing polymerization of reboiler gas phase dead zone in styrene rectification process |
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| CN1109861A (en) * | 1995-03-11 | 1995-10-11 | 天津大学北方化工新技术开发公司 | Rectifying device for refining crude vanillin |
| US5799510A (en) * | 1997-07-30 | 1998-09-01 | The Boc Group, Inc. | Multi-column system and method for producing pressurized liquid product |
| CN2389156Y (en) * | 1999-08-06 | 2000-07-26 | 陈丽文 | Rosin rectifying equipment |
| CN101070277A (en) * | 2007-06-18 | 2007-11-14 | 厦门金达威维生素股份有限公司 | Method and apparatus for purifying vitamin A intermediate mynistic aldehyde |
| WO2008046626A2 (en) * | 2006-10-18 | 2008-04-24 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
| CN201880386U (en) * | 2010-10-19 | 2011-06-29 | 常州吉恩化工有限公司 | Rectifying device |
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2010
- 2010-10-19 CN CN201010510541A patent/CN101961562B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109861A (en) * | 1995-03-11 | 1995-10-11 | 天津大学北方化工新技术开发公司 | Rectifying device for refining crude vanillin |
| US5799510A (en) * | 1997-07-30 | 1998-09-01 | The Boc Group, Inc. | Multi-column system and method for producing pressurized liquid product |
| CN2389156Y (en) * | 1999-08-06 | 2000-07-26 | 陈丽文 | Rosin rectifying equipment |
| WO2008046626A2 (en) * | 2006-10-18 | 2008-04-24 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
| CN101070277A (en) * | 2007-06-18 | 2007-11-14 | 厦门金达威维生素股份有限公司 | Method and apparatus for purifying vitamin A intermediate mynistic aldehyde |
| CN201880386U (en) * | 2010-10-19 | 2011-06-29 | 常州吉恩化工有限公司 | Rectifying device |
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Owner name: CHANGZHOU GENCHEM + GENPHARM PHARMACEUTICAL CO., L Free format text: FORMER NAME: CHANGZHOU JIEN CHEMICAL CO.,LTD. |
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Address after: 213127 No. 658 ERON North Road, Xinbei District, Jiangsu, Changzhou Patentee after: GENCHEM & GENPHARM (CHANGZHOU) CO., LTD. Address before: 213127, Jiangsu, Hebei Province, Changzhou north side of the river chemical industry park, west of new Dai Road, south of the Port Road, Changzhou Jean Chemical Co., Ltd. Patentee before: Changzhou Jien Chemical Co.,Ltd. |