CN102430381B - Carbonylation reacting kettle - Google Patents
Carbonylation reacting kettle Download PDFInfo
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- CN102430381B CN102430381B CN201110289090.7A CN201110289090A CN102430381B CN 102430381 B CN102430381 B CN 102430381B CN 201110289090 A CN201110289090 A CN 201110289090A CN 102430381 B CN102430381 B CN 102430381B
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Abstract
The invention relates to a carbonylation reacting kettle, comprising a kettle body, and a separation plate which is arranged in the kettle body and used for separating the kettle body to form an upstream and a downstream area of which the two ends communicates with each other. A liquid outlet is arranged on the bottom part of the kettle body, and a gas outlet is arranged on the top part of the kettle body. A liquid inlet and a liquid distributor are arranged on the upper part of the kettle body. A liquid jetting opening of the liquid distributor of which at least one opening faces upwards is arranged in the upstream or located in the vertical extending area of the upstream which faces the top part, and a liquid jetting opening of the liquid distributor of which at least one opening faces downwards is arranged in the downstream area or located in the vertical extending area of the downstream area which faces the top part. A gas inlet and a gas distributor are arranged on the lower part of the kettle body. A gas jetting micro-pore of the gas distributor is located in the upstream or located in the vertical extending area of the upstream which faces the bottom part, and the opening faces upwards. The arrangement position of the liquid distributor is higher than that of the gas distributor.
Description
Technical field
The present invention relates to a kind of carbonylation still, belong to chemical industry equipment field.
Background technology
Acetic acid and acetic anhydride are important Organic Chemicals, are widely used as the raw material of medicine, dyestuff, spices and organic synthesis, their the synthetic general method that adopts carbonylation of industry.Being specially and adopting methyl alcohol, CO is that raw material and catalyst carry out carbonylation and obtain acetic acid; Take methyl acetate, methyl alcohol and carbon monoxide as raw material, and under the effect of rhodium series catalysts, reaction makes aceticanhydride.
Because the carbonylation of acetic acid and acetic anhydride is heterogeneous chemical reaction, for reactant is mixed, the general reactor adopting with agitator, but because the reactor sealing with agitator is poor, expend the energy large, and not quick detachable and affect extent of reaction after generation fault, therefore in recent years adopt the reactor without agitating device to carry out carbonylation more.
The above-mentioned carbonylation still without agitator, such as Japan Patent JP8188547A, it discloses a kind of internal-circulation type carbonylation still, comprises kettle, has the inner core of a cylindrical both ends open in kettle; Autoclave body bottom and be positioned at described inner core below be provided with liquid-inlet, gas feed and nozzle, on the top of kettle, be provided with and catalyst carried out from liquid to separated separation chamber, the liquid reaction product after separation is discharged from arranging with the liquid outlet of described separation chamber sidewall; In addition top, ， separation chamber is also provided with gas vent, and gas vent connects condenser; Carbonylation still in this technology is when operation, catalyst is distributed in reactor in advance, by liquid-inlet and gas nozzle, in inner core, import liquids and gases, liquids and gases drive catalyst to flow, thereby in inner core, form catalyst, gas and the liquid mobile mixture fluid that makes progress, gap location between kettle and inner core forms downward fluid, thereby form on the whole the mobile circulation of feed liquid, finally, product is discharged by liquid outlet after separation chamber's separation, and the tail gas of unreacted gas and generation is discharged by gas vent.
In above-mentioned technology, due in this reactor, the outlet of gas and liquid is all arranged on the bottom of inner core, reactant mixture during work in inner core need to move upward under gas raw material makes progress the drive of jet power, but when the jet power of gas raw material is not enough, can not effectively drive reactant mixture to move up to the top of inner core, more cannot realization response mixture from inner core top carrying out smoothly of circulation downwards.
Summary of the invention
Technical problem to be solved by this invention is the bottom that the outlet of carbonylation still gas of the prior art and liquid is all arranged on inner core, reactant mixture during work in inner core need to move upward under gas raw material makes progress the drive of jet power, but when the jet power of gas raw material is not enough, can not effectively drive reactant mixture to move up to the top of inner core, more cannot realization response mixture from inner core top carrying out smoothly of circulation downwards; And then a kind of carbonylation still that can form the circulation of reactant mixture fast and effectively in reactor proposed.
For solving the problems of the technologies described above, the invention provides a kind of carbonylation still, it comprises:
Kettle, connects the dividing plate being arranged in described kettle described kettle is separated into up district and the descender that two ends communicate; On described kettle, be provided with liquid-inlet, liquid outlet and gas feed, top is provided with gas vent; Be connected with described liquid-inlet, in described kettle, be provided with liquid distribution trough, described liquid distribution trough is provided with liquid ejection outlet; Be connected with described gas feed, in described kettle, be provided with gas distributor, described gas distributor is provided with gas and sprays micropore; The setting position of described liquid distribution trough is higher than described gas distributor, at least one first liquid jet of described liquid distribution trough is positioned at described up district or is positioned at described up district towards the district extending longitudinally at top, and at least one second liquid jet of liquid distribution trough is positioned at described descender or is positioned at described descender towards the district extending longitudinally at top; The opening upwards of described first liquid jet, Open Side Down for described second liquid jet; The gas of described gas distributor sprays micropore and is positioned at described up district or is positioned at described up district towards the district extending longitudinally of bottom, and described gas sprays the opening upwards of micropore.
The setting position of described liquid distribution trough is not higher than the top of described dividing plate, and the setting position of described gas distributor is not less than the bottom of described dividing plate.
Described dividing plate axis centered by the axis of described kettle is cylindrical around being connected to form.
The gas of described gas distributor sprays micropore and is symmetrical arranged centered by the axis of described kettle.
Described first liquid jet is symmetrical arranged centered by the axis of described kettle, and described second liquid jet is symmetrical arranged centered by the axis of described kettle.
Described dividing plate is arc-shaped surface, described dividing plate is connected with described inner wall of kettle, from upper end and the described kettle joint of described dividing plate, start downward-sloping first opening section that is provided with, from the lower end of described dividing plate and described kettle joint, starting to be inclined upwardly is provided with the second opening section.
The angle of described the first opening section and described kettle axis is 20-90 °.
Described angle is 45 °.
The angle of described the second opening section and described kettle axis is 20-90 °.
Described angle is 60 °.
Wherein, to spray micropore described in micropore be that the diameter of finger-hole reaches micron order for gas of the present invention.
The diameter that described gas sprays micropore is 5-20 micron.
The present invention compares and has following beneficial effect with prior art scheme:
(1) in carbonylation still of the present invention, the setting position of described liquid distribution trough is higher than described gas distributor, at least one first liquid jet of described liquid distribution trough is positioned at described up district or is positioned at described up district and (dividing plate extended vertically towards the district extending longitudinally at top, extended dividing plate is divided into the district extending longitudinally in up district and the district extending longitudinally of descender by kettle) in, and at least one second liquid jet of liquid distribution trough is positioned at described descender or is positioned at described descender towards the district extending longitudinally at top; The opening upwards of described first liquid jet, Open Side Down for described second liquid jet; The gas of described gas distributor sprays micropore and is positioned at described up district or is positioned at described up district towards the district extending longitudinally of bottom, and described gas sprays the opening upwards of micropore; liquid charging stock and liquid catalyst are input in kettle by liquid-inlet and liquid ejection outlet, simultaneously gas raw material sprays micropore by gas feed and gas and is input to up district or up district in the district extending longitudinally at top, gas sprays pore openings upwards, the gas of ejection forms uniform reactant mixture and reacts after mixing with the liquid in up district or up district district extending longitudinally, and reactant mixture motion from bottom to top under the drive of gas injection micropore jet power, in the time of near reaching up district or the up district first liquid jet in the district extending longitudinally at top, the jet power that first liquid jet makes progress can supplement provides power to drive reactant mixture to continue to move upward, when reactant mixture enters into descender or descender when the district extending longitudinally at top is moved downward by the impact of gravity, the liquid charging stock being sprayed by second liquid jet and liquid catalyst supplement in reactant mixture, for carbonylation provides new reactant, simultaneously the downward jet power of second liquid jet provides power to drive reactant mixture to move downward to get back to up district or up district continues to participate in reaction and circulates in the district extending longitudinally of bottom, and then make reactant mixture in kettle, form circulation fast and effectively.
(2) in carbonylation still of the present invention, the setting position of described liquid distribution trough is not higher than the top of described dividing plate, and the setting position of described gas distributor is not less than the bottom of described dividing plate; Reactant mixture up district and descender extend axially district in carry out circulation time, owing to there is no the isolation of dividing plate, up with descending reactant mixture easily meets and mixes and jet power is up or down offseted, thereby weak the carrying out of circulation, the circulation of reactant mixture is limited to the generation of having avoided this situation between up district and descender, and shortened the range ability circulating, accelerated the carrying out of circulation.
(3) in carbonylation still of the present invention, described dividing plate axis centered by the axis of described kettle is cylindrical around being connected to form, the gas of described gas distributor sprays micropore and is symmetrical arranged centered by the axis of described kettle, described first liquid jet is symmetrical arranged centered by the axis of described kettle, and described second liquid jet is symmetrical arranged centered by the axis of described kettle; Between up district and descender, circulating in all directions of reactant mixture evenly carried out, thereby guaranteed reactant mixture being evenly distributed in up district, in whole up district, all can carry out carbonylation, improved efficiency and the productive rate of reaction.
(4) in carbonylation still of the present invention, described dividing plate is arc-shaped surface, described dividing plate is connected with described inner wall of kettle, from upper end and the described kettle joint of described dividing plate, start downward-sloping first opening section that is provided with, from the lower end of described dividing plate and described kettle joint, starting to be inclined upwardly is provided with the second opening section.The inwall of described dividing plate and kettle joins kettle is divided into up district and descender, saved like this manufactured materials of reactor, and facilitate finishing and the cleaning of zones of different in kettle, downward-sloping and acclivitous opening section makes reactant mixture shorten at the cycling distance of up district and downlink interval, thereby without very large power, just can form the circulation of reactant mixture, circulation is more easily realized.
Accompanying drawing explanation
For content of the present invention is more easily understood, the present invention is further detailed content of the present invention with the specific embodiment by reference to the accompanying drawings;
Fig. 1 is that the carbonylation still of the embodiment of the present invention one is along the profile of axis;
Fig. 2 is that the carbonylation still of the embodiment of the present invention two is along the profile of axis;
Fig. 3 is the front view of the carbonylation still of the embodiment of the present invention three;
Fig. 4 is the top view of the carbonylation still of the embodiment of the present invention three;
Wherein Reference numeral is: 1-kettle, and 2-dividing plate, 3-gas vent, 4-liquid-inlet, 5-liquid ejection outlet, 6-gas feed, 7-gas sprays micropore, 8-liquid outlet, 9-support bar, 10-circular arc region, 11-the first opening section, 12-the second opening section.
The specific embodiment
Embodiment mono-
Carbonylation still structure of the present invention as shown in Figure 1, comprise: kettle 1, in described kettle 1 inside, be provided with dividing plate 2, described dividing plate 2 axis centered by the axis of described kettle 1 surrounds cylindrical around connection, the support bar 9 that described dividing plate 2 is connected on kettle 1 sidewall by 4 symmetries is fixed, the cylindrical region that described dividing plate 2 surrounds is descender, between described dividing plate 2 outer walls and kettle 1 inwall, form up district, up district communicates with the two ends of descender, described kettle 1 is 1.5-2 with the internal diameter ratio of descender, kettle 1 bottom is provided with liquid outlet 8, the liquid generating for discharging reaction, the top of kettle 1 is provided with gas vent 3, be used for discharging reaction end gas and unreacted gas, on the top of kettle 1, be provided with a liquid-inlet 4, for infusion fluid reaction raw materials and liquid catalyst, the liquid distribution trough that liquid-inlet 4 along continuous straight runs are connected with pallet shape extend in kettle 1, the height of liquid distribution trough is lower than dividing plate 2 upper end 100-200mm, liquid distribution trough is arranged with the liquid ejection outlet 5 of 8 opening upwards in up district centered by kettle 1 axis, and centered by kettle 1 axis, is arranged with 5 liquid ejection outlets that Open Side Down 5 in descender, in the bottom of kettle 1, be provided with a gas feed 6, be used for inputting gas raw material, gas feed 6 be positioned at liquid-inlet 4 under, the gas distributor that gas feed 6 along continuous straight runs are connected with pallet shape extend in kettle 1, gas distributor be positioned at liquid distribution trough under, the height of gas distributor is higher than dividing plate 2 lower end 100-200mm, and the gas that gas distributor is arranged with 8 opening upwards in up district centered by kettle 1 axis sprays micropore 7.
Embodiment bis-
Carbonylation still structure described in the present embodiment as shown in Figure 2, comprise: the cylindrical region that described dividing plate 2 surrounds is up district, between described dividing plate 2 outer walls and kettle 1 inwall, form descender, up district communicates with the two ends of descender, described kettle 1 is 1.5-2 with the internal diameter ratio in up district, liquid distribution trough is arranged with the liquid ejection outlet 5 of 5 opening upwards in up district centered by kettle 1 axis, and in descender, centered by kettle 1 axis, be arranged with 4 liquid ejection outlets that Open Side Down 5, the gas that gas distributor is arranged with 5 opening upwards in up district centered by kettle 1 axis sprays micropore 7, the structure of remainder is identical with embodiment mono-.
Embodiment tri-
Carbonylation still structure described in the present embodiment as shown in Figure 3,4, comprise: kettle 1, in described kettle 1, there is a dividing plate 2 that is arc-shaped surface to be connected with described kettle 1 inwall, from upper end and kettle 1 joint of dividing plate 2, start downward-sloping formation the first opening section 11 simultaneously, described the first opening section 11 is 45 ° with the angle of kettle 1 axis, and from the lower end of described dividing plate 2 and described kettle 1 joint, starting to be inclined upwardly forms the second opening section 12, and described the second opening section 12 is 60 ° with the angle of kettle 1 axis, the 10Wei descender, circular arc region that described dividing plate 2 inwalls and described kettle 1 inwall surround, the region that described dividing plate 2 outer walls and described kettle 1 inwall form is up district, up district communicates with the two ends of descender, liquid-inlet 4 along continuous straight runs are connected with linear liquid distribution trough and extend in kettle 1, the height of liquid distribution trough is lower than dividing plate 2 upper end 100-200mm, liquid distribution trough is provided with the liquid ejection outlet 5 of 1 opening upwards in up district, and in descender, be provided with 1 liquid ejection outlet that Open Side Down 5, gas feed 6 along continuous straight runs are connected with linear gas distributor and extend in up district, gas distributor be positioned at liquid distribution trough under, the height of gas distributor is higher than dividing plate 2 lower end 100-200mm, the gas that gas distributor is provided with 2 opening upwards in up district sprays micropore 7, the structure of remainder is identical with embodiment mono-.
Gas described in above-described embodiment sprays micropore 7 can select any micron-sized diameter according to actual needs, and wherein preferred micro-pore diameter is 5-20 micron.
The course of work of carbonylation still of the present invention is as follows:
Liquid charging stock and liquid catalyst are input in kettle 1 by liquid-inlet 4 and liquid ejection outlet 5, gas raw material is input in up district by gas feed 6 and gas injection micropore 7 simultaneously, gas sprays micropore 7 opening upwards, and the gas of ejection mixes the uniform reactant mixture of rear formation and reacts with the liquid in up district, reactant mixture sprays micropore 7 at gas and upwards under the drive of jet power, moves upward, in the time of near reactant mixture moves to the liquid ejection outlet 5 in up district, due to liquid ejection outlet 5 opening upwards in up district, the jet power that liquid ejection outlet 5 makes progress drives reactant mixture to continue to move upward, until move downward behind the top of arrival descender, the liquid charging stock of the downward liquid ejection outlet of descender split shed 5 ejections and liquid catalyst are carbonylation provides fresh reactant, simultaneously the downward jet power of liquid ejection outlet 5 provides power for the motion of reactant mixture in descender, drive reactant mixture motion from top to bottom in descender, until flow out descender, enter continuation participation reaction and circulation in up district, between up district in kettle 1 and descender, formed thus the circulation of reactant mixture, the incorporation time that has extended reactant makes reactant mixture more even, improved the utilization rate of reactant, improved productive rate simultaneously.
Although the present invention elaborates it by above-mentioned specific embodiment; but; those skilled in the art should be understood that any form that does not exceed claim protection domain made on this basis and the variation of details, all belong to invention which is intended to be protected.
Claims (1)
1. a carbonylation still, comprising:
Kettle (1),
Connect the dividing plate (2) being arranged in described kettle (1) described kettle (1) is separated into up district and the descender that two ends communicate;
On described kettle (1), be provided with liquid-inlet (4), liquid outlet (8) and gas feed (6), top is provided with gas vent (3);
Be connected with described liquid-inlet (4), in described kettle (1), be provided with liquid distribution trough, described liquid distribution trough is provided with liquid ejection outlet (5);
Be connected with described gas feed (6), in described kettle (1), be provided with gas distributor, described gas distributor is provided with gas and sprays micropore (7);
It is characterized in that,
The setting position of described liquid distribution trough is higher than described gas distributor, at least one first liquid jet (5) of described liquid distribution trough is positioned at described up district or is positioned at described up district towards the district extending longitudinally at top, and at least one second liquid jet (5) of liquid distribution trough is positioned at described descender or is positioned at described descender towards the district extending longitudinally at top;
The opening upwards of described first liquid jet (5), Open Side Down for described second liquid jet (5);
The gas of described gas distributor sprays micropore (7) and is positioned at described up district or is positioned at described up district towards the district extending longitudinally of bottom, and described gas sprays the opening upwards of micropore (7).
2. carbonylation still according to claim 1, is characterized in that, the setting position of described liquid distribution trough is not higher than the top of described dividing plate (2), and the setting position of described gas distributor is not less than the bottom of described dividing plate (2).
3. carbonylation still according to claim 1 and 2, is characterized in that, described dividing plate (2) axis centered by the axis of described kettle (1) is cylindrical around being connected to form.
4. carbonylation still according to claim 3, is characterized in that, the gas of described gas distributor sprays micropore (7) and is symmetrical arranged centered by the axis of described kettle (1).
5. according to the carbonylation still described in claim 1 or 2 or 4, it is characterized in that, described first liquid jet (5) is symmetrical arranged centered by the axis of described kettle (1), and described second liquid jet (5) is symmetrical arranged centered by the axis of described kettle (1).
6. carbonylation still according to claim 1 and 2, it is characterized in that, described dividing plate (2) is arc-shaped surface, described dividing plate (2) is connected with described kettle (1) inwall, from upper end and described kettle (1) joint of described dividing plate (2), start downward-sloping the first opening section (11) that is provided with, from the lower end of described dividing plate (2) and described kettle (1) joint, starting to be inclined upwardly is provided with the second opening section (12).
7. carbonylation still according to claim 6, is characterized in that, described the first opening section (11) is 20-90 ° with the angle of described kettle (1) axis.
8. carbonylation still according to claim 7, is characterized in that, described angle is 45 °.
9. according to the carbonylation still described in claim 7 or 8, it is characterized in that, described the second opening section (12) is 20-90 ° with the angle of described kettle (1) axis.
10. carbonylation still according to claim 9, is characterized in that, described angle is 60 °.
11. according to the carbonylation still described in claim 1 or 2 or 4 or 7 or 8 or 10, it is characterized in that, the diameter that described gas sprays micropore (7) is 5-20 micron.
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| CN201110289090.7A CN102430381B (en) | 2011-09-27 | 2011-09-27 | Carbonylation reacting kettle |
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| CN201110289090.7A CN102430381B (en) | 2011-09-27 | 2011-09-27 | Carbonylation reacting kettle |
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| CN102430381B true CN102430381B (en) | 2014-01-22 |
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| CN104028178B (en) * | 2013-03-06 | 2016-03-02 | 中石化上海工程有限公司 | The method of fortified water mechanics reactor mixed effect |
| CN111362792A (en) * | 2019-09-12 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Enhanced reaction system and process for preparing acetic acid by methanol carbonylation |
| CN111389321A (en) * | 2020-03-23 | 2020-07-10 | 山东凯泰科技股份有限公司 | Reactor for producing chloropropene |
| CN113499739A (en) * | 2021-07-16 | 2021-10-15 | 南京延长反应技术研究院有限公司 | DMC preparation system and method for instant dehydration |
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| DE3206661A1 (en) * | 1982-02-25 | 1983-09-01 | Basf Ag, 6700 Ludwigshafen | METHOD FOR AVOIDING AN EXPLOSIBLE GAS PHASE IN GAS / LIQUID REACTIONS |
| US5243083A (en) * | 1992-07-24 | 1993-09-07 | Texaco Chemical Company | Thermosyphonic reaction of oxygen with isobutane and reactor |
| DE4237369A1 (en) * | 1992-11-05 | 1994-05-11 | Salzgitter Anlagenbau | Gas=liquid reactor for methyl formate prepn. - with improved dispersion of carbon mon:oxide, higher conversion and lower energy input. |
| JP2972904B2 (en) * | 1994-12-29 | 1999-11-08 | 千代田化工建設株式会社 | Carbonylation reaction method and reactor |
| US5883292A (en) * | 1996-01-17 | 1999-03-16 | Twenty-First Century Research Corporation | Reaction control by regulating internal condensation inside a reactor |
| US5767303A (en) * | 1996-10-04 | 1998-06-16 | Chiyoda Corporation | Process of producing carbonic diester |
| DE19854637A1 (en) * | 1998-11-26 | 2000-05-31 | Basf Ag | Reactor for the continuous implementation of gas-liquid, liquid-liquid or gas-liquid-solid reactions |
| CN1291925C (en) * | 2004-11-30 | 2006-12-27 | 东南大学 | Horizontal integrated three phase inner circulation fluidized reactor and its biological reaction process |
| CN201592098U (en) * | 2010-01-18 | 2010-09-29 | 富艺国际工程有限公司 | Jet loop reactor for preparing polyoxyethylene ester |
| CN101885678B (en) * | 2010-07-05 | 2013-03-13 | 兖矿国泰化工有限公司 | Reaction equipment for synthesizing ethylic acid by low-pressure methanol carbonylation of methanol |
| CN202238060U (en) * | 2011-09-27 | 2012-05-30 | 陕西煤业化工技术开发中心有限责任公司 | Carbonylation reaction kettle |
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