CN103157425A - 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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- CN103157425A CN103157425A CN2011104142741A CN201110414274A CN103157425A CN 103157425 A CN103157425 A CN 103157425A CN 2011104142741 A CN2011104142741 A CN 2011104142741A CN 201110414274 A CN201110414274 A CN 201110414274A CN 103157425 A CN103157425 A CN 103157425A
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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 for adopting phase transfer catalyst to carry out the continuous producing apparatus of catalytic reaction.
Technical background
In catalytic reaction process, although homogeneous catalysis has the advantages such as reactivity is high, reaction condition is gentle, because being difficult to recycle, its catalyst limited it in industrial application.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 reaction, because being dissolved in reaction system, a kind of effect of substrate wherein carries out homogeneous catalytic reaction in reaction, after reaction finishes, when this exhausted substrate, catalyst can be separated out from reaction system again, can recycle (science by separating, 2001, 292, 1139), the phospho heteropoly tungstate that wherein has reaction control phase transfer characteristics has good activity in epoxidation reaction of olefines, the process of its catalysis hydrogen peroxide oxidation cyclohexene 7-oxa-bicyclo[4.1.0 processed has realized industrialization (Mechanisms in homogeneous and heterogeneous epoxidation catalysis ISBN:978-0-444-53188-9 2008). but because catalyst must be through separating, therefore can't realize serialization production.For the type catalyst, we have invented the continuous reaction equipment that is suitable for having in reaction mass the solid particle slurries, need not in reaction product and catalyst are advanced isolated by filtration and reslurry with slurry material process, realized the continued operation of reaction control phase transfer catalyst catalytic process, this consersion unit is suitable equally for the liquid phase reaction course that generally has common heterogeneous catalyst simultaneously.
Summary of the invention
A kind of continuous producing apparatus for adopting phase-transfer-catalyzed reactions, described equipment is connected in series by overflow pipe by I stage reactor and II stage reactor, material enters in the I stage reactor continuously by charging aperture, advance the II stage reactor through overflow pipe again, isolate continuously clear liquid after crossing filter core finally by the metal sintering of II stage reactor upper end, the serum materials that contains solid particle by slurry reflux pipeline continuous backflow to the 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 mouth, liquid level gauge mouth, condensate liquid import; The safety relief mouth is equipped with at the cylindrical shell top, and cylindrical shell band heating/cooling jacket is equipped with water inlet and delivery port on the chuck layer; In the II stage reactor, metal sintering is housed and crosses filter core; Slip reflux inlet, discharging opening are equipped with 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 proportion of the diameter of cylinder and height is 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 ℃, and working pressure is between 0～10.0MPa, and solid particle accounts for proportion in serum materials between 0～30%.
Described deflection plate quantity is evenly distributed on reactor wall between 2～6.
Described gas distributor can be the pore formula or the metal sintering pipe is crossed filer element type, and gas distributor is arranged on I stage reactor and II stage reactor inner bottom part, and installation direction is vertical with the reactor axial direction.
It is consistent that metal sintering in the clear liquid discharging opening quantity of described II stage reactor and II stage reactor is crossed filter core quantity, clear liquid discharging opening setting height(from bottom) require II stage reactor cylindrical shell height 75～80% between, the installation site evenly distributes on same level in drum shaft.
Described cylinder body bottom is equipped with gas feed.
Described thermometer mouth is that multiple spot distributes, and requires each reactor to control the monitoring number of fragments between 2～12.
Described pressure gauge mouth installation requirement is more than the liquid level face.
Be equipped with described I stage reactor bottom the slip reflux inlet.
The setting height(from bottom) of described I stage reactor discharging opening require the reactor cylinder height 75～80% between.
Described II stage reactor charging aperture is positioned at the bottom of II stage reactor.
Described slurries outlet is positioned under the clear liquid discharging opening, and quantity is between 2～8.
The 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 are equipped with water inlet and delivery port on the chuck layer, chuck quantity is between 2～8 groups.
The present invention has following advantage:
Present device can satisfy the characteristics that the employing phase transfer catalyst carries out catalytic reaction, realized the serialization production of such catalytic reaction, overcome the operation at intermittence of such catalytic reaction of tradition, greatly shorten its technological process, having saved to contain needs the operating procedure that filter, again prepare burden, pull an oar after the solid particle slurry reaction, and provides condition for the industrially scalable maximization of such catalytic reaction.
Description of drawings
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;
The wherein symbolic representation in accompanying drawing 1:
The 1-I stage reactor; The 2-II stage reactor; The 3-agitator; The 4-deflection plate; The 5-gas distributor; The 6-sintering is crossed filter core; The 7-discharging opening; The 8-gas feed; 9-slurry reflux entrance; The 10-condenser; The 13-charging aperture; The 14-discharging opening; The 15-charging aperture; 16-stillness of night discharging opening; 18-safety relief mouth; 19-thermometer mouth; The 21-motor; 22-heating/cooling jacket; 23-chuck water inlet; 24-chuck delivery port; The 25-overflow pipe; 26-pressure gauge mouth; 27-liquid level gauge mouth; The import of 28-condensate liquid; The 29-slurry outlet.
The specific embodiment
The below will be described in detail patent of the present invention by specific embodiment, but it is only to explain rather than limit patent of the present invention.
Adopt equipment shown in Figure 1, the height H of I stage reactor and II stage reactor cylinder is 3000mm, diameter is 500mm, the deflection plate height H is 2400mm, with the distance of reactor cylinder inwall be 100mm, quantity is 4, gas distributor adopts sintered metal tube to cross filer element type, it is 20mm that metal sintering filters core diameter, and hole is selected 0.5 μ m, and quantity is 4.
Carry out reaction-controlled phase transfer catalysis hydrogen peroxide direct oxidation chloropropene epoxychloropropane processed.
Hydrogen peroxide enters in reactor from I stage reactor 3,1 top charging aperture 13 continuously, 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 enters the interior continuation reaction of II level stage reactor 2 by overflow pipe, product is from reactor 2 stillness of night outlet 16 continuous discharges, and the reaction paste that contains solid catalyst particle is got back in I stage reactor 1 from backflow of slurry mouth 29 by the slurry measuring pump.
The apparatus and process condition is as follows:
Reaction temperature is 44 ℃, keeps reactor pressure as 0.3MPa take the nitrogen continuous feed, and speed of agitator is controlled at 300 rev/mins, and the 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 referring to Journal of Molecular Catalysis A, 2001,166:219., and the catalyst particles granularity is between 1～50 μ m, and catalyst is in disposable input reactor in advance.
Isolated clear liquid analysis is obtained the conversion ratio of selective, hydrogen peroxide of yield, the epoxychloropropane of epoxychloropropane.
Claims (7)
1. one kind is used for adopting phase transfer catalyst to carry out the continuous producing apparatus of catalytic reaction, it is characterized in that:
Comprise I stage reactor (1) and II stage reactor (2);
Be provided with charging aperture (13) on the side wall surface of I stage reactor (1);
Be provided with discharging opening (14) on the middle and upper part side wall surface of I stage reactor (1);
Be provided with charging aperture (15) on the lower sides of II reactor (2);
Discharging opening (14) is connected 15 with charging aperture) connect by overflow pipe (25);
Be provided with on the upper side wall of II stage reactor (2) and contain the built-in clear liquid discharging opening (16) of crossing filter core (6);
Be provided with slurry reflux entrance (9) on the lower sides of I stage reactor (1), be provided with slurries outlets (29) on the middle and upper part sidewall of II stage reactor (2);
Slurry reflux outlet (29) is connected 9 with the slurry reflux entrance) connect by pipeline, and be provided with mashing pump on their connecting pipe.
2. continuous producing apparatus according to claim 1 is characterized in that:
Be provided with agitator (3) in I stage reactor (1) and II stage reactor (2), be provided with deflection plate (4) on I stage reactor (1) and II stage reactor (2) internal face, be provided with gas distributor (5) in I stage reactor (1) and II stage reactor (2) inner bottom part, gas distributor (5) is connected with extraneous source of the gas by gas distributor interface (8).
3. continuous producing apparatus according to claim 1 is characterized in that:
Be provided with pressure gauge mouth (26), liquid level gauge mouth (27), thermometer mouth (19) on the side wall surface of I stage reactor (1) and II stage reactor (2);
Top in I stage reactor (1) and II stage reactor (2) is provided with safety relief mouth (18);
Be provided with discharging opening (7) in I stage reactor (1) and II stage reactor (2) bottom.
4. continuous producing apparatus according to claim 1, it is characterized in that: in all bands heating/cooling jacket (22) of I stage reactor (1) and II stage reactor (2), be provided with chuck water inlet (23) and chuck delivery port (24) on heating/cooling jacket (22).
5. continuous producing apparatus according to claim 1 is characterized in that:
Be equipped with in described II stage reactor (2) cross filter core (6), be that detachable pipeline is connected with reactor-side wall supernatant discharging opening (16) connected mode, the mistake filter core is that metal sintering is crossed filter core;
The hole that metal sintering is crossed filter core (6) requires between 0.1～100 μ m, quantitative requirement is between 2～32, metal sintering is crossed filter core (6) and is shaped as the open circles column type, and the internal diameter of diameter and II stage reactor (2) requires proportion between 1: 4～12;
The setting height(from bottom) of described I stage reactor (1) and II stage reactor (2) require consistent or I stage reactor (1) bottom higher than II stage reactor (2) bottom between 1～50%.
6. continuous producing apparatus according to claim 1 is characterized in that:
Described agitator (3) is in transmission connection with motor (21); Described agitator (3) is Multi-stage stirring, and progression is between 2～15.
7. continuous producing apparatus according to claim 1, it is characterized in that: described I stage reactor (1) and II stage reactor (2) top are provided with speeds to exit condenser (10), 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 liquid entrance (28) of reactor, and the condensate liquid entrance (28) of reactor requires more than the liquid level of reactor.
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| Application Number | Priority Date | Filing Date | Title |
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| 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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| 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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| CN103157425B 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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Granted publication date: 20150107 Termination date: 20191213 |