CN102430381A - Carbonylation reacting kettle - Google Patents
Carbonylation reacting kettle Download PDFInfo
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- CN102430381A CN102430381A CN2011102890907A CN201110289090A CN102430381A CN 102430381 A CN102430381 A CN 102430381A CN 2011102890907 A CN2011102890907 A CN 2011102890907A CN 201110289090 A CN201110289090 A CN 201110289090A CN 102430381 A CN102430381 A CN 102430381A
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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 the 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, the synthetic general method that adopts carbonylation of their industry.Being specially and adopting methyl alcohol, CO is that raw material and catalyst carry out carbonylation and obtain acetic acid; With methyl acetate, methyl alcohol and carbon monoxide is raw material, and reaction makes aceticanhydride under the effect of rhodium series catalysts.
Because the carbonylation of acetic acid and acetic anhydride is a heterogeneous chemical reaction; For reactant is mixed; The general agitated reactor that has agitator that adopts, but owing to the agitated reactor sealing that has agitator is poor, it is big to expend the energy; And not quick detachable and influence extent of reaction after the generation fault, therefore in recent years adopt the agitated reactor of no agitating device to carry out carbonylation more.
The carbonylation still of above-mentioned no agitator, such as Japan Patent JP8188547A, it discloses a kind of internal-circulation type carbonylation still, comprises kettle, and the inner core of a cylindrical both ends open is arranged in the kettle; Autoclave body bottom and be positioned at said inner core below be provided with liquid-inlet, gas feed and nozzle; Be provided with on the top of kettle catalyst is carried out extracts and fractions from liquid, the liquid reaction product after the separation is discharged from being provided with the liquid outlet of said separation chamber sidewall; In addition, also be provided with gas vent at the top, separation chamber, gas vent connects condenser; Carbonylation still in this technology is when operation; Catalyst is distributed in the agitated reactor in advance, in inner core, imports liquids and gases by liquid-inlet and gas nozzle, and liquids and gases drive catalyst and flow; Thereby in inner core, form the mixture fluid that catalyst, gas and liquid upwards flow; Gap location between kettle and inner core forms downward fluid, thereby constitutes the circulation that feed liquid flows on the whole, and is last; Product is discharged by liquid outlet after the separation chamber separates, and the tail gas of unreacted gas and generation is discharged by gas vent.
In the above-mentioned technology; Because in this agitated reactor; The outlet of gas and liquid all is arranged on the bottom of inner core; Reactant mixture during work in the inner core need 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, then can not drive the top that reactant mixture moves up to inner core effectively, more can't the realization response mixture from the 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 all is arranged on inner core; Reactant mixture during work in the inner core need 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, then can not drive the top that reactant mixture moves up to inner core effectively, more can't the realization response mixture from the inner core top carrying out smoothly of circulation downwards; And then a kind of carbonylation still that can in agitated reactor, form the circulation of reactant mixture fast and effectively 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 that is arranged in the said kettle said kettle is separated into up district and the descender that two ends communicate; On said kettle, be provided with liquid-inlet, liquid outlet and gas feed, the top is provided with gas vent; Be connected with said liquid-inlet, in said kettle, be provided with liquid distribution trough, said liquid distribution trough is provided with liquid ejection outlet; Be connected with said gas feed, in said kettle, be provided with gas distributor, said gas distributor is provided with gas and sprays micropore; The position that is provided with of said liquid distribution trough is higher than said gas distributor; At least one of said liquid distribution trough first liquid ejection outlet is positioned at said up district or is positioned at the longitudinal extension district of said up district towards the top, and at least one second liquid ejection outlet of liquid distribution trough is positioned at said descender or is positioned at the longitudinal extension district of said descender towards the top; The opening of said first liquid ejection outlet makes progress, and Open Side Down for said second liquid ejection outlet; The gas of said gas distributor sprays micropore and is positioned at said up district or is positioned at the longitudinal extension district of said up district towards the bottom, and the opening that said gas sprays micropore makes progress.
Said liquid distribution trough the top that the position is not higher than said dividing plate is set, said gas distributor the bottom that the position is not less than said dividing plate is set.
Said dividing plate is that central axis is cylindrical around being connected to form with the axis of said kettle.
The gas injection micropore of said gas distributor is that the center is symmetrical set with the axis of said kettle.
Said first liquid ejection outlet is that the center is symmetrical set with the axis of said kettle, and said second liquid ejection outlet is that the center is symmetrical set with the axis of said kettle.
Said dividing plate is an arc-shaped surface; Said dividing plate is connected with said inner wall of kettle; Begin downward-sloping first opening section that is provided with from the upper end and the said kettle joint of said dividing plate, beginning to be inclined upwardly from the lower end of said dividing plate and said kettle joint is provided with second opening section.
The angle of said first opening section and said kettle axis is 20-90 °.
Said angle is 45 °.
The angle of said second opening section and said kettle axis is 20-90 °.
Said angle is 60 °.
Wherein, to spray micropore described in the micropore be that the diameter of finger-hole reaches micron order for gas of the present invention.
The diameter that said gas sprays micropore is the 5-20 micron.
The present invention compares with the prior art scheme has following beneficial effect:
(1) in the carbonylation still of the present invention; The position that is provided with of said liquid distribution trough is higher than said gas distributor; At least one of said liquid distribution trough first liquid ejection outlet is positioned at said up district or is positioned at said up district and (dividing plate extended vertically towards the longitudinal extension district at top; Extended dividing plate is divided into the longitudinal extension district in up district and the longitudinal extension district of descender with kettle) in, and at least one second liquid ejection outlet of liquid distribution trough is positioned at said descender or is positioned at the longitudinal extension district of said descender towards the top; The opening of said first liquid ejection outlet makes progress, and Open Side Down for said second liquid ejection outlet; The gas of said gas distributor sprays micropore and is positioned at said up district or is positioned at the longitudinal extension district of said up district towards the bottom, and the opening that said gas sprays micropore makes progress; Liquid charging stock and liquid catalyst are input in the 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 longitudinal extension district at top; Gas sprays pore openings upwards; The uniform reactant mixture of formation and reacting after gas and the liquid mixing in up district or the longitudinal extension district, up district of ejection; 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 up district first liquid ejection outlet in the longitudinal extension district at top; The jet power that first liquid ejection outlet makes progress can replenish provides power drive reactant mixture to continue to move upward; When reactant mixture enters into descender or descender when the longitudinal extension district at top is moved downward by the influence of gravity, replenish in the reactant mixture, for carbonylation provides new reactant by the liquid charging stock of second liquid ejection outlet ejection and liquid catalyst; Simultaneously the downward jet power of second liquid ejection outlet provides power to drive reactant mixture to move downward and get back to up district or up district continues to participate in reaction and circulation in the longitudinal extension district of bottom, and then reactant mixture has been formed fast and effectively circulate in kettle.
(2) in the carbonylation still of the present invention, said liquid distribution trough the top that the position is not higher than said dividing plate is set, said gas distributor the bottom that the position is not less than said dividing plate is set; Reactant mixture carries out circulation time extending axially of up district and descender in the district; Owing to there is not the isolation of dividing plate; Up with descending reactant mixture meets easily and mixes and jet power is up or down offseted, thereby more weak the carrying out of circulation is limited to the generation of having avoided this situation between up district and the descender with the circulation of reactant mixture; And shortened the range ability that circulates, accelerated the carrying out of circulation.
(3) in the carbonylation still of the present invention; Said dividing plate is that central axis is cylindrical around being connected to form with the axis of said kettle; The gas injection micropore of said gas distributor is that the center is symmetrical set with the axis of said kettle; Said first liquid ejection outlet is that the center is symmetrical set with the axis of said kettle, and said second liquid ejection outlet is that the center is symmetrical set with the axis of said kettle; Circulating on all directions of reactant mixture evenly carried out between up district and the descender, thereby guaranteed reactant mixture being evenly distributed in up district, in whole up district, all can carry out carbonylation, improved the efficient and the productive rate of reaction.
(4) in the carbonylation still of the present invention; Said dividing plate is an arc-shaped surface; Said dividing plate is connected with said inner wall of kettle; Begin downward-sloping first opening section that is provided with from the upper end and the said kettle joint of said dividing plate, beginning to be inclined upwardly from the lower end of said dividing plate and said kettle joint is provided with second opening section.The inwall of said dividing plate and kettle joins kettle is divided into up district and descender; Saved the manufactured materials of agitated reactor like this; And make things convenient for the finishing and the cleaning of zones of different in the kettle; Downward-sloping and acclivitous opening section makes reactant mixture shorten at the cycling distance of up district and downlink interval, thereby need not the circulation that very big power just can constitute reactant mixture, makes that circulation more is prone to realize.
Description of drawings
For content of the present invention is understood more easily, the present invention combines the accompanying drawing and the specific embodiment that content of the present invention is further explained;
Fig. 1 is the profile of the carbonylation still of the embodiment of the invention one along axis;
Fig. 2 is the profile of the carbonylation still of the embodiment of the invention two along axis;
Fig. 3 is the front view of the carbonylation still of the embodiment of the invention three;
Fig. 4 is the vertical view of the carbonylation still of the embodiment of the invention three;
Wherein Reference numeral is: the 1-kettle, and the 2-dividing plate, the 3-gas vent, the 4-liquid-inlet, the 5-liquid ejection outlet, the 6-gas feed, 7-gas sprays micropore, 8-liquid outlet, 9-support bar, 10-circular arc zone, 11-first opening section, 12-second opening section.
The specific embodiment
Embodiment one
Carbonylation still structure of the present invention is as shown in Figure 1, comprising: kettle 1 has dividing plate 2 in said kettle 1 set inside; It is cylindrical that said dividing plate 2 is with the axis of said kettle 1 that central axis surrounds around connection; Said dividing plate 2 is fixed through the support bar 9 that 4 symmetries are connected on kettle 1 sidewall, and the cylindrical region that said dividing plate 2 surrounds is a descender, forms up district between said dividing plate 2 outer walls and kettle 1 inwall; Up district communicates with the two ends of descender; Said kettle 1 is 1.5-2 with the internal diameter ratio of descender, and kettle 1 bottom is provided with liquid outlet 8, is used to discharge the liquid that reaction generates; The top of kettle 1 is provided with gas vent 3, is used to discharge reaction end gas and unreacted gas; Be provided with a liquid-inlet 4 on the top of kettle 1; Be used to import liquid reaction raw material and liquid catalyst; The liquid distribution trough that liquid-inlet 4 along continuous straight runs are connected with pallet shape extend in the kettle 1; The height of liquid distribution trough is lower than dividing plate 2 upper end 100-200mm, and liquid distribution trough is that the center is arranged with the liquid ejection outlet 5 that 8 openings make progress with kettle 1 axis in up district, and in descender, is that the center is arranged with 5 liquid ejection outlets that Open Side Down 5 with kettle 1 axis; Be provided with a gas feed 6 in the bottom of kettle 1; Be used to import 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 the 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 gas distributor is that the center is arranged with the gas that 8 openings make progress and sprays micropore 7 with kettle 1 axis in up district.
Embodiment two
The described carbonylation still of present embodiment structure is as shown in Figure 2; Comprise: the cylindrical region that said dividing plate 2 surrounds is up district; Form descender between said dividing plate 2 outer walls and kettle 1 inwall; Up district communicates with the two ends of descender, and the internal diameter in said kettle 1 and up district is than being 1.5-2, and liquid distribution trough is that the center is arranged with the liquid ejection outlet 5 that 5 openings make progress with kettle 1 axis in up district; And in descender, be that the center is arranged with 4 liquid ejection outlets that Open Side Down 5 with kettle 1 axis, gas distributor is that the center is arranged with the gas that 5 openings make progress and sprays micropore 7 with kettle 1 axis in up district; The structure of remainder is identical with embodiment one.
Embodiment three
The described carbonylation still of present embodiment structure is like Fig. 3, shown in 4; Comprise: kettle 1; Have in the said kettle 1 one be arc-shaped surface dividing plate 2 be connected with said kettle 1 inwall; Upper end and kettle 1 joint from dividing plate 2 begins downward-sloping formation first opening section 11 simultaneously; Said first opening section 11 is 45 ° with the angle of kettle 1 axis, and begins to be inclined upwardly with said kettle 1 joint from the lower end of said dividing plate 2 and form second opening section 12, and the angle of said second opening section 12 and kettle 1 axis is 60 °; The circular arc zone 10 that said dividing plate 2 inwalls and said kettle 1 inwall surround is descender; The zone that said dividing plate 2 outer walls and said kettle 1 inwall form is up district; Up district communicates with the two ends of descender, and liquid-inlet 4 along continuous straight runs are connected with linear liquid distribution trough and extend in the kettle 1, and 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 that 1 opening makes progress 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 the 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, and gas distributor is provided with the gas injection micropore 7 that 2 openings make progress in up district; The structure of remainder is identical with embodiment one.
Gas described in the foregoing description sprays micropore 7 can select any micron-sized diameter according to actual needs, and wherein preferred micro-pore diameter is the 5-20 micron.
The course of work of carbonylation still of the present invention is following:
Liquid charging stock and liquid catalyst are input in the kettle 1 by liquid-inlet 4 and liquid ejection outlet 5; Gas raw material is input in the up district by gas feed 6 and gas injection micropore 7 simultaneously; Gas sprays micropore 7 openings upwards, the uniform reactant mixture of formation and reacting after the liquid mixing in the gas of ejection and the up district; Reactant mixture sprays micropore 7 at gas and upwards moves upward under the drive of jet power; In the time of near reactant mixture moves to the liquid ejection outlet 5 in the up district; Because liquid ejection outlet 5 openings in the up district upwards, the jet power that liquid ejection outlet 5 makes progress drives reactant mixture to be continued to move upward, and behind the top that arrives descender, moves downward; The liquid charging stock of the downward liquid ejection outlet of descender split shed 5 ejections and the liquid catalyst fresh reactant that has been providing of carbonylation; Liquid ejection outlet 5 downward jet powers are that the motion of reactant mixture in descender provides power simultaneously, drive reactant mixture motion from top to bottom in descender, get into until the outflow descender and continue in the up district to participate in reaction and circulate; Formed the circulation of reactant mixture thus between up district in kettle 1 and the descender; The incorporation time that has prolonged reactant makes reactant mixture more even, has improved the utilization rate of reactant, has improved productive rate simultaneously.
Though the present invention has carried out detailed elaboration through above-mentioned specific embodiment to it; But; Any form that does not exceed the claim protection domain that those skilled in the art should be understood that on this basis to be made and the variation of details all belong to invention which is intended to be protected.
Claims (11)
1. carbonylation still agitated reactor comprises:
Kettle (1),
Connect the dividing plate (2) that is arranged in the said kettle (1) said kettle (1) is separated into up district and the descender that two ends communicate;
On said kettle (1), be provided with liquid-inlet (4), liquid outlet (8) and gas feed (6), the top is provided with gas vent (3);
Be connected with said liquid-inlet (4), in said kettle (1), be provided with liquid distribution trough, said liquid distribution trough is provided with liquid ejection outlet (5);
Be connected with said gas feed (6), in said kettle (1), be provided with gas distributor, said gas distributor is provided with gas and sprays micropore (7);
It is characterized in that,
The position that is provided with of said liquid distribution trough is higher than said gas distributor; At least one of said liquid distribution trough first liquid ejection outlet (5) is positioned at said up district or is positioned at the longitudinal extension district of said up district towards the top, and at least one second liquid ejection outlet (5) of liquid distribution trough is positioned at said descender or is positioned at the longitudinal extension district of said descender towards the top;
The opening of said first liquid ejection outlet (5) makes progress, and Open Side Down for said second liquid ejection outlet (5);
The gas of said gas distributor sprays micropore (7) and is positioned at said up district or is positioned at the longitudinal extension district of said up district towards the bottom, and the opening that said gas sprays micropore (7) makes progress.
2. carbonylation still agitated reactor according to claim 1 is characterized in that, said liquid distribution trough the top that the position is not higher than said dividing plate (2) is set, said gas distributor the bottom that the position is not less than said dividing plate (2) is set.
3. carbonylation still according to claim 1 and 2 is characterized in that, said dividing plate (2) is that central axis is cylindrical around being connected to form with the axis of said kettle (1).
4. according to the arbitrary described carbonylation still of claim 1-3, it is characterized in that the gas injection micropore (7) of said gas distributor is that the center is symmetrical set with the axis of said kettle (1).
5. according to the arbitrary described carbonylation still of claim 1-4; It is characterized in that; Said first liquid ejection outlet (5) is that the center is symmetrical set with the axis of said kettle (1), and said second liquid ejection outlet (5) is that the center is symmetrical set with the axis of said kettle (1).
6. carbonylation still according to claim 1 and 2; It is characterized in that; Said dividing plate (2) is an arc-shaped surface; Said dividing plate (2) is connected with said kettle (1) inwall, begins downward-sloping first opening section (11) that is provided with from the upper end and said kettle (1) joint of said dividing plate (2), begins to be inclined upwardly from the lower end of said dividing plate (2) and said kettle (1) joint to be provided with second opening section (12).
7. carbonylation still according to claim 6 is characterized in that, said first opening section (11) is 20-90 ° with the angle of said kettle (1) axis.
8. carbonylation still according to claim 7 is characterized in that, said angle is 45 °.
9. according to claim 6 or 7 or 8 described carbonylation stills, it is characterized in that said second opening section (12) is 20-90 ° with the angle of said kettle (1) axis.
10. carbonylation still according to claim 9 is characterized in that, said angle is 60 °.
11., it is characterized in that the diameter that said gas sprays micropore (7) is the 5-20 micron according to the arbitrary described carbonylation still of claim 1-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN102430381A true CN102430381A (en) | 2012-05-02 |
| CN102430381B CN102430381B (en) | 2014-01-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028178A (en) * | 2013-03-06 | 2014-09-10 | 中石化上海工程有限公司 | Method for reinforcing mixing effect of hydraulic reactor |
| CN111389321A (en) * | 2020-03-23 | 2020-07-10 | 山东凯泰科技股份有限公司 | Reactor for producing chloropropene |
| WO2021047056A1 (en) * | 2019-09-12 | 2021-03-18 | 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 means of carbonylation methanol |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104028178A (en) * | 2013-03-06 | 2014-09-10 | 中石化上海工程有限公司 | Method for reinforcing mixing effect of hydraulic reactor |
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| WO2021047056A1 (en) * | 2019-09-12 | 2021-03-18 | 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 means of carbonylation methanol |
| 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 |
| WO2023284030A1 (en) * | 2021-07-16 | 2023-01-19 | 南京延长反应技术研究院有限公司 | Instant dewatering dmc preparation system and preparation method |
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|---|---|
| CN102430381B (en) | 2014-01-22 |
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