CN103157425B - Continuous production device for catalytic reaction by adopting phase transfer catalyst - Google Patents
Continuous production device for catalytic reaction by adopting phase transfer catalyst Download PDFInfo
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- CN103157425B CN103157425B CN201110414274.1A CN201110414274A CN103157425B CN 103157425 B CN103157425 B CN 103157425B CN 201110414274 A CN201110414274 A CN 201110414274A CN 103157425 B CN103157425 B CN 103157425B
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Abstract
The invention discloses a continuous production device for catalytic reaction by adopting a phase transfer catalyst. The continuous production device can meet the catalytic reaction which is carried out through the phase transfer catalyst. The continuous production device is composed of multi-grade reactors connected in serials. Raw materials continuously enter a grade-I reactor through a feeding port, a reaction mixture and a catalyst enter a grade-II reactor through an overflow port, a sintering metal filter core which is installed on the upper end of a secondary reactor continuously filters and separates clean liquid, and serum containing solid particles continuously returns into the grade-I reactor to be continuously reacted through a serum backflow pipeline via an outlet at the bottom of the secondary reactor. By adopting the continuous production device, continuous operation of the phase transfer catalyst catalytic reaction is realized.
Description
Technical field
Patent of the present invention relates to a kind of chemical production equipment, is specifically related to a kind of continuous producing apparatus for adopting phase transfer catalyst to carry out catalytic reaction.
Technical background
In catalytic reaction process, although homogeneous catalysis has the advantages such as reactivity is high, reaction condition is gentle, limit its application industrially because its catalyst is difficult to recycle.Reaction control phase transfer catalyst is the new catalyst that a class has the advantage of homogeneous catalyst and heterogeneous catalyst concurrently, it is solid before the reaction, be dissolved in reaction system due to the effect of wherein a kind of substrate in reaction and carry out homogeneous catalytic reaction, after reaction terminates, when this exhausted substrate, catalyst can be separated out again from reaction system, (science can be recycled by being separated, 2001, 292, 1139), the phospho heteropoly tungstate wherein with reaction-controlled phase-transfer feature has good activity in epoxidation reaction of olefines, the process of its catalysis hydrogen peroxide oxidation cyclohexene 7-oxa-bicyclo[4.1.0 has realized industrialization (Mechanisms in homogeneous and heterogeneous epoxidation catalysis ISBN:978-0-444-53188-9 2008). but have to pass through separation due to catalyst, therefore continuous prodution cannot be realized.For the type catalyst, we have invented the continuous reaction equipment being suitable for having in reaction mass solid particle slurries, without the need to product and catalyst being entered isolated by filtration and reslurry joins slurry process in reaction, achieve the continued operation of reaction control phase transfer catalyst catalytic process, this consersion unit is applicable equally for the liquid phase reaction course generally with common heterogeneous catalyst simultaneously.
Summary of the invention
A kind of for adopting the continuous producing apparatus of phase-transfer-catalyzed reactions, described equipment is connected in series by overflow pipe by I stage reactor and II stage reactor, material enters in I stage reactor by charging aperture continuously, II stage reactor is entered again through overflow pipe, be continuously separated out clear liquid after metal sintering filtration core finally by II stage reactor upper end, the serum materials containing solid particle passes through slurry reflux pipeline continuous backflow in I stage reactor; I stage reactor and II stage reactor are equipped with agitator, deflection plate, gas distributor, discharge port, air inlet, thermometer mouth, pressure gauge port, liquid level gauge mouth, condensate liquid import; Safety relief mouth is equipped with at cylindrical shell top, and cylindrical shell band heating/cooling jacket, chuck layer is equipped with water inlet and delivery port; II stage reactor is built with metal sintering filtration core; Slip reflux inlet is equipped with, discharging opening in I stage reactor side; Charging aperture is equipped with in II stage reactor side, clear liquid discharging opening, slurry outlet.
Described I stage reactor (1) and II stage reactor are cylindrical shape, and the diameter of cylinder and the proportion of height are between 1: 1.5 ~ 15, and the top of cylinder and bottom air-tight manner adopt flange form airtight.I stage reactor and II stage reactor volume ratio scope are between 1: 1 ~ 3, and I stage reactor volume is at 0.1m
3~ 30m
3between.
Described serviceability temperature is between 0 ~ 200 DEG C, and use pressure between 0 ~ 10.0MPa, solid particle accounts for proportion in serum materials between 0 ~ 30%.
Described deflection plate quantity, between 2 ~ 6 pieces, is evenly distributed on reactor wall.
Described gas distributor can be Tube hole type or metal sintering pipe filters core type, and gas distributor is arranged on I stage reactor and II stage reactor inner bottom part, and installation direction is vertical with reactor axial direction.
The clear liquid discharging opening quantity of described II stage reactor is consistent with the metal sintering filtration core quantity in II stage reactor, clear liquid discharging opening setting height(from bottom) requires between 75 ~ 80% of II stage reactor cylindrical shell height, and installation site is uniformly distributed in same level in drum shaft.
Described cylinder body bottom is equipped with gas feed.
Described thermometer mouth is multiple spot distribution, requires that each reactor controls monitoring number of fragments between 2 ~ 12.
Described pressure gauge port installation requirement is more than liquid level face.
What be equipped with bottom described I stage reactor has slip reflux inlet.
The setting height(from bottom) of described I stage reactor discharging opening requires between 75 ~ 80% of reactor cylinder height.
Described II stage reactor charging aperture is positioned at the bottom of II stage reactor.
Under described serum outlet is positioned at clear liquid discharging opening, quantity is between 2 ~ 8.
Safety relief mouth is equipped with at described I stage reactor and II stage reactor cylindrical shell top.
Described I stage reactor and II stage reactor cylindrical shell band Segmented heating/cooling jacket, chuck layer is equipped with water inlet and delivery port, chuck quantity is between 2 ~ 8 groups.
Tool of the present invention has the following advantages:
Present device can meet the feature adopting phase transfer catalyst to carry out catalytic reaction, achieve the continuous prodution of such catalytic reaction, overcome the intervalization operation of such catalytic reaction of tradition, greatly shorten its technological process, eliminate the operating procedure containing needing after solid particle slurry reaction to filter, again prepare burden, pull an oar, and for such catalytic reaction industrially scalable maximize provide condition.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, patent of the present invention is further detailed.
Fig. 1 is the equipment schematic diagram of phase-transfer-catalyzed reactions;
Symbol wherein in accompanying drawing 1 represents:
1-I stage reactor; 2-II stage reactor; 3-agitator; 4-deflection plate; 5-gas distributor; The sintered filter core of 6-; 7-discharging opening; 8-gas feed; 9-slurry reflux entrance; 10-condenser; 13-charging aperture; 14-discharging opening; 15-charging aperture; 16-stillness of night discharging opening; 18-safety relief mouth; 19-thermometer mouth; 21-motor; 22-heating/cooling jacket; 23-chuck water inlet; 24-chuck delivery port; 25-overflow pipe; 26-pressure gauge port; 27-liquid level gauge mouth; The import of 28-condensate liquid; 29-slurry outlet.
Detailed description of the invention
To be described in detail patent of the present invention by specific embodiment below, but it is only explain instead of limit patent of the present invention.
Embodiment 1
The equipment shown in Fig. 1 of employing, the height H of I stage reactor and II stage reactor cylinder is 3000mm, diameter is 500mm, deflection plate height H is 2400mm, is 100mm with the distance of reactor cylinder inwall, and quantity is 4 pieces, gas distributor adopts sintered metal tube to filter core type, metal sintering filtration core diameter is 20mm, and hole selects 0.5 μm, and quantity is 4.
Carry out reaction-controlled phase transfer catalysis hydrogen peroxide direct oxidation chloropropene epoxychloropropane.
Hydrogen peroxide enters in reactor continuously from 3, I stage reactor 1 top charging aperture 13, chloropropene enters reactor continuously by I stage reactor 1 underfeed mouth 13, nitrogen enters in reaction system by the gas distributor 5 of I stage reactor 1 and II stage reactor 2, reaction mass in I level stage reactor 1 is entered in II level stage reactor 2 by overflow pipe and continues reaction, product exports 16 continuous discharges from reactor 2 stillness of night, and the reaction paste containing solid catalyst particle is got back in I stage reactor 1 from backflow of slurry mouth 29 by slurry measuring pump.
Apparatus and process condition is as follows:
Reaction temperature is 44 DEG C, and maintain reactor pressure for 0.3MPa with nitrogen continuous feed, speed of agitator controls at 300 revs/min, and chloropropene inlet amount is 10L/ hour, and 50% hydrogen peroxide inlet amount is 2L/ hour.
Catalyst is a kind of phosphotungstic acid quaternary, and its preparation method is see Journal of Molecular Catalysis A, 2001,166:219., and catalyst particle size is between 1 ~ 50 μm, and catalyst is in advance in disposable input reactor.
Isolated clear liquid analysis is obtained to the conversion ratio of selective, hydrogen peroxide of the yield of epoxychloropropane, epoxychloropropane.
Claims (4)
1. the continuous producing apparatus for adopting phase transfer catalyst to carry out catalytic reaction, is characterized in that:
Comprise I stage reactor (1) and II stage reactor (2);
Charging aperture I (13) is provided with on the side wall surface of I stage reactor (1);
Discharging opening I (14) is provided with on the middle and upper part side wall surface of I stage reactor (1);
Charging aperture II (15) is provided with on the lower sides of II stage reactor (2);
Discharging opening I (14) is connected by overflow pipe (25) with charging aperture II (15);
The clear liquid discharging opening (16) containing built-in filtration core (6) is provided with on the upper side wall of II stage reactor (2);
On the lower sides of I stage reactor (1), be provided with slurry reflux entrance (9), on the middle and upper part sidewall of II stage reactor (2), be provided with slurry reflux outlet (29);
Slurry reflux outlet (29) is connected by pipeline with slurry reflux entrance (9), and is provided with mashing pump in their connecting pipe;
Agitator (3) is provided with in I stage reactor (1) and II stage reactor (2), deflection plate (4) is provided with on I stage reactor (1) and II stage reactor (2) internal face, I stage reactor (1) and II stage reactor (2) inner bottom part are provided with gas distributor (5), and gas distributor (5) is connected with extraneous source of the gas by gas distributor interface (8);
Pressure gauge port (26), liquid level gauge mouth (27), thermometer mouth (19) is provided with on the side wall surface of I stage reactor (1) and II stage reactor (2);
Safety relief mouth (18) is provided with in the top of I stage reactor (1) and II stage reactor (2);
Discharging opening II (7) is provided with in I stage reactor (1) and II stage reactor (2) bottom;
Periodic off-gases condenser (10) is provided with in I stage reactor (1) and II stage reactor (2) top, condenser (10) upper end is connected with gas discharge line and control valve, the condensate outlet of lower end is connected by pipeline with the condensate inlet (28) of reactor, and the condensate inlet (28) of reactor requires more than the liquid level of reactor.
2. continuous producing apparatus according to claim 1, it is characterized in that: I stage reactor (1) and II stage reactor (2), all with heating/cooling jacket (22), heating/cooling jacket (22) are provided with chuck water inlet (23) and chuck delivery port (24).
3. continuous producing apparatus according to claim 1, is characterized in that:
Described II stage reactor (2) built with filtration core (6), be that detachable pipeline is connected with reactor-side wall supernatant discharging opening (16) connected mode, filtration core is metal sintering filtration core;
The hole of metal sintering filtration core (6) requires between 0.1 ~ 100 μm, and quantitative requirement is between 2 ~ 32, and metal sintering filtration core (6) shape is hollow cylindrical;
The setting height(from bottom) of described I stage reactor (1) and II stage reactor (2) requires bottom consistent or I stage reactor (1) higher than II stage reactor (2) bottom.
4. continuous producing apparatus according to claim 1, is characterized in that:
Described agitator (3) and motor (21) are in transmission connection; Described agitator (3) is Multi-stage stirring, and progression is between 2 ~ 15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110414274.1A CN103157425B (en) | 2011-12-13 | 2011-12-13 | Continuous production device for catalytic reaction by adopting phase transfer catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110414274.1A CN103157425B (en) | 2011-12-13 | 2011-12-13 | Continuous production device for catalytic reaction by adopting phase transfer catalyst |
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| CN103157425A CN103157425A (en) | 2013-06-19 |
| CN103157425B true CN103157425B (en) | 2015-01-07 |
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Citations (8)
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| DE19622840A1 (en) * | 1996-06-07 | 1997-12-11 | Episucres Sa | Continuous liquid phase reaction with heterogeneous catalyst in a pulsed column |
| CN1186716A (en) * | 1997-10-28 | 1998-07-08 | 北京燕山石油化工公司研究院 | Continuous stirring polymerizing reactor tower |
| CN101230114A (en) * | 2008-01-04 | 2008-07-30 | 中国寰球工程公司 | Polymerization reactor and method for producing polypropylene by employing the same |
| CN201670810U (en) * | 2010-03-19 | 2010-12-15 | 中国石油天然气股份有限公司 | Device for synthesizing dicarboxylate through multiple-kettle serial connection and continuous deep esterification |
| CN101992055A (en) * | 2010-11-03 | 2011-03-30 | 天津大学 | Method and device of continuously synthesizing tetramethyl ammonium carbonate by multi-reactors in series |
| CN201793508U (en) * | 2010-08-12 | 2011-04-13 | 上海氯碱化工股份有限公司 | Device for producing dichloroethane |
| CN102166505A (en) * | 2011-03-22 | 2011-08-31 | 江苏中丹集团股份有限公司 | Resorcinol alkali fusion workshop section reaction device and reaction technology thereof |
| CN202343197U (en) * | 2011-12-13 | 2012-07-25 | 中国科学院大连化学物理研究所 | Continuous production device for catalytic reaction adopting phase transfer catalyst |
-
2011
- 2011-12-13 CN CN201110414274.1A patent/CN103157425B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19622840A1 (en) * | 1996-06-07 | 1997-12-11 | Episucres Sa | Continuous liquid phase reaction with heterogeneous catalyst in a pulsed column |
| CN1186716A (en) * | 1997-10-28 | 1998-07-08 | 北京燕山石油化工公司研究院 | Continuous stirring polymerizing reactor tower |
| CN101230114A (en) * | 2008-01-04 | 2008-07-30 | 中国寰球工程公司 | Polymerization reactor and method for producing polypropylene by employing the same |
| CN201670810U (en) * | 2010-03-19 | 2010-12-15 | 中国石油天然气股份有限公司 | Device for synthesizing dicarboxylate through multiple-kettle serial connection and continuous deep esterification |
| CN201793508U (en) * | 2010-08-12 | 2011-04-13 | 上海氯碱化工股份有限公司 | Device for producing dichloroethane |
| CN101992055A (en) * | 2010-11-03 | 2011-03-30 | 天津大学 | Method and device of continuously synthesizing tetramethyl ammonium carbonate by multi-reactors in series |
| CN102166505A (en) * | 2011-03-22 | 2011-08-31 | 江苏中丹集团股份有限公司 | Resorcinol alkali fusion workshop section reaction device and reaction technology thereof |
| CN202343197U (en) * | 2011-12-13 | 2012-07-25 | 中国科学院大连化学物理研究所 | Continuous production device for catalytic reaction adopting phase transfer catalyst |
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