CN101747163A - Process for simulative continuous counter-current absorption of ketene by acetone - Google Patents
Process for simulative continuous counter-current absorption of ketene by acetone Download PDFInfo
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- CN101747163A CN101747163A CN200810204711A CN200810204711A CN101747163A CN 101747163 A CN101747163 A CN 101747163A CN 200810204711 A CN200810204711 A CN 200810204711A CN 200810204711 A CN200810204711 A CN 200810204711A CN 101747163 A CN101747163 A CN 101747163A
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Abstract
The invention relates to a process for the simulative continuous counter-current absorption of ketene by acetone, which is characterized in that: at least three reactors are arranged, wherein reaction materials, namely the acetone and catalysts are added into the reactors; two reactors are connected in series for reaction and another one reactor is for later use; the three reactors are switched to perform operation in turn; a stirring paddle of each reactor adopts a closed-type bent-blade disk turbine paddle; the simulative continuous counter-current absorption of the ketene is realized through negative pressure; a condenser and a gas-liquid separator are arranged at the back stage of each reactor; gas phase generated during the reaction of the reactors is condensed by the condenser and separated by the gas-liquid separator; and liquid phase flows back to the reactors and the gas phase enters the next-stage reactor. The process has the advantages that: the ketene is absorbed by the negative pressure which is generated by stirring the closed-type bent-blade disk turbine paddle, so the ketene gas delivery pressure and the autopolymerization reaction are reduced, the stirring efficiency is high, and the dispersion effect is good even if thickened catalysts such as ASA and the like exist. A plurality of reactors can be connected in series when necessary to form a certain concentration gradient so as to realize the counter-current absorption.
Description
Technical field
The present invention relates to a kind of process for simulative continuous counter-current absorption of ketene by acetone.
Background technology
Ketene is a kind of compound of high value, make by acetic acid or acetone Pintsch process, under different catalyst actions, absorb fine chemical product such as the isopropenyl acetate that afterreaction can make high added value through acetone, methyl ethyl diketone, dimethacrylate etc., but ketene character is extremely active, and severe toxicity arranged, easy polymerization under the pressurized conditions, traditional acetone technology adopts the single still of periodical operation to absorb more, this technology ketene absorbs not exclusively, fluctuation of operating conditions, the needs of incompatibility scale operation are so the continuously complete absorption technique exploitation of ketene is an emphasis and difficult point always.
English Patent GB717827 has proposed to adopt the series connection of two stills, also stream absorbs ketene technology continuously, the ketene transmitting power mainly relies between this technological reaction still increases the ketene transfer pressure, because ketene is along with pressure increases, polymerization side reactions is also along with increase, this must cause the ketene transformation efficiency low, particularly the transmitting power of the second still ketene is lower, simultaneously, owing to adopt and the stream absorption, the second still ketene concentration is low, and the acetone material concentration is also lower, causes assimilation effect poor, and ketene absorbs not exclusively, final ketene transformation efficiency only reaches 68%, caused the significant wastage of ketene and the difficulty of exhaust aftertreatment technology, resulting absorption liquid production concentration is also lower, and separation costs is higher.
English Patent GB965607 has proposed to adopt the spiral pipe reactor continuous absorption ketene technology of absorption tower or strap clamp cover, this process system resistance is big, need increase the ketene feed gas pressure greatly, because ketene itself is autohemagglutination easily, has caused this technology can only be applicable to that ketene content is lower than 10% exhaust treatment system.
Chinese patent CN200610051620.3 has proposed the esterification column absorption technique, single esterification column periodical operation, two esterification columns switch in turn, it is low that the single esterification column of this technology absorbs the later stage acetone concentration, assimilation effect is poor, simultaneously, the catalyzer that this technology was suitable for also has certain limitation, to thickness catalyzer such as the extraordinary ASA of present acetone ketene effect because of the obstruction that easily causes esterification column with disperse inhomogeneous can't the application.
Summary of the invention
The purpose of this invention is to provide that a kind of ketene gas transfer pressure is low, self-polymeric reaction is few, dispersion effect good, be suitable for the process for simulative continuous counter-current absorption of ketene by acetone of thickness catalyzer.
The technical scheme of taking for achieving the above object is: a kind of process for simulative continuous counter-current absorption of ketene by acetone, it is characterized by: 3 reactors are set at least, add reaction mass acetone and catalyzer in the described reactor, absorb flow process and adopt 2 still cascade reactions, 1 still is awaited orders, and 3 stills take turns blocked operation; The reactor stirring rake adopts closed curved leaf disc turbine oar, and negative pressure realizes that the simulation continuous countercurrent of ketene absorbs; The back level of described reactor is equipped with condenser and gas-liquid separator, and the gas phase that produces in the reactor reaction process is through condenser condenses, gas-liquid separator separates, the described reactor of liquid-phase reflux, gas phase enters the next stage reactor, absorbs back tail gas and sends into the flare system processing.
Specifically, described a kind of process for simulative continuous counter-current absorption of ketene by acetone:
1) ketene is delivered to the 1st still that series connection absorbs by the cracking operation, regulate the 1st still rotating speed of agitator, produce the negative pressure of 0～40kPa, suck ketene, under sufficient stirring and catalyst action, reaction heat is emitted in the ketene rapid reaction simultaneously, along with reaction is carried out, acetone steam and a small amount of unreacted ketene gas rise, through condenser condenses and gas-liquid separator separates, liquid phase is returned the 1st still, and gas phase enters the 2nd still;
2) the 2nd still reaction of series connection absorption is regulated the 2nd still rotating speed of agitator with the 1st still, produces the negative pressure of 0～40kPa, suck the remaining ketene gas in the 1st still reaction back, consider that the ketene gas concentration that enters is very low, reaction heat is less, suitably improves the needed temperature of reaction; Acetone steam and a spot of non-condensable gases such as CO
2, CH
4Deng through condenser condenses and gas-liquid separator separates, liquid phase is returned the 2nd still, the gas phase gas processing system that truncates;
3) standby still is got acetone and catalyzer ready, keeps suitable temperature, can cut at any time as reactor;
4) the 1st still reacts to production concentration and reaches institute when requiring concentration, cuts out as standby still, emit reaction solution after, get the raw materials ready again, add acetone and catalyzer, keep suitable temperature;
5) when the 1st still cuts out as standby still, the 2nd still switches simultaneously as the 1st still, and former standby still switches as the 2nd still;
6) so move in circles, realize the continuous absorption of ketene.
Described reactor cylinder inboard wall is equipped with longitudinal baffle, and the reactor cylindrical shell outside is equipped with chuck.
Be equipped with the stirring rake blade on the stir shaft of described closed curved leaf disc turbine oar.
Described reactor quantity is the 3-6 platform, realizes many stills cascade reaction.
After described standby still adds acetone and catalyzer, 30～60 ℃ of preheating temperatures, standby.
Described reactor control reaction temperature is 40～100 ℃.
Advantage of the present invention is: the reactor stirring rake has adopted closed curved leaf disc turbine oar, adopts this stirring rake, can be when stirring, the disc turbine center produces stronger negative pressure, with the ketene suction, thereby reduce the ketene gas transfer pressure, reduced self-polymeric reaction; Provide transmitting power in particular for small amount of ethylene ketone transfer of gas between reactor and the reactor; Adopt this stirring rake, make the ketene gas of suction throw away along the disk radial direction, prevent that gas from passing through stirring rake wheel hub low shear zone on every side through turbine oar whirlpool shape passage, the stirring efficiency height, dispersion effect is good; Further, install common stirring rake blade on the stir shaft additional, strengthen gas dispersion, help reaction to carry out rapidly and uniformly by adding baffle plate at the reactor cylinder inboard wall; Adopt this stirring rake to stir, guaranteed also can obtain good dispersion effect when thickness compound such as ASA is made catalyzer.
Another significant advantage of the present invention is: realized ketene simulation continuous countercurrent absorption process, it is bigger to enter the 1st still ketene concentration, this moment, acetone concentration was lower, the ketene density loss after absorbing through the 1st still, and the acetone concentration of the 2nd still is higher relatively, guaranteed the abundant absorption of ketene, since adopted closed curved leaf disc turbine oar to guarantee the transmitting power of ketene, under the situation of needs, many stills of can also connecting, form certain concentration gradient, thereby realize counter-current absorption.
Description of drawings
Fig. 1 simulative continuous counter-current absorption of ketene by acetone prepares the isopropenyl acetate process flow diagram.Among the figure, R1, R2, R3 are respectively reactor, and E1, E2, E3 are condenser, and S1, S2, S3 are gas-liquid separator, and A1 is common blade, and A2 is closed curved leaf disc turbine oar, and A3 is a baffle plate.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Figure 1 shows that a kind of simulative continuous counter-current absorption of ketene by acetone prepares the isopropenyl acetate technical process.Be example to adopt 3 reactors (R1, R2, R3) among the figure, concrete technical process is: add reaction mass acetone and catalyzer in the described reactor, absorb flow process and adopt 2 still cascade reactions, 1 still is awaited orders, and 3 stills take turns blocked operation; The reactor stirring rake adopts closed curved leaf disc turbine oar A2, and negative pressure realizes that the simulation continuous countercurrent of ketene absorbs; The back level of described reactor is equipped with condenser E and gas-liquid separator S, and the gas phase that produces in the reactor reaction process is through condenser E condensation, gas-liquid separator S separates, the described reactor of liquid-phase reflux, gas phase enters the next stage reactor, absorbs back tail gas and sends into the flare system processing.
Specifically, described a kind of process for simulative continuous counter-current absorption of ketene by acetone:
1) ketene is delivered to the 1st still R1 that series connection absorbs by the cracking operation, regulate the 1st still R1 stirring rake A2 rotating speed to 200 commentaries on classics/min, produce the negative pressure of 17kPa, suck ketene, under sufficient stirring and catalyst action, the ketene rapid reaction, emit reaction heat simultaneously, control reaction temperature is 40～100 ℃, preferred 65 ℃, along with reaction is carried out, acetone steam and a small amount of unreacted ketene gas rise, condensation separates with gas-liquid separator S1 through condenser E1, and liquid phase is returned the 1st still R1, and gas phase enters the 2nd still R2;
2) the 2nd still R2 reaction of series connection absorption is with the 1st still R1, regulate the 2nd still R2 rotating speed of agitator to 200 commentaries on classics/min, produce 17kPa negative pressure, suck the remaining ketene gas in the 1st still R1 reaction back, consider that the ketene gas concentration that enters is very low, reaction heat is less, suitably improves the needed temperature of reaction, react and feed steam in the 2nd still chuck and suitably heat, keep that reaction system is little boils; Acetone steam and a spot of non-condensable gases such as CO
2, CH
4Deng condensation separates with gas-liquid separator S2 through condenser E2, liquid phase is returned the 2nd still R2, the gas phase gas processing system that truncates;
3) standby still R3 gets acetone and catalyzer ready, and preheating temperature is 30～60 ℃, and 40 ℃ of preferred temperature can be cut at any time as reactor;
4) the 1st still R1 reacts to product isopropenyl acetate concentration and reaches at 83% o'clock, cuts out as standby still, emit reaction solution by the 1st still R1 bottom after, get the raw materials ready again, add acetone and catalyzer, keep 40 ℃ of temperature;
5) when the 1st still R1 cuts out as standby still, the 2nd still R2 switches simultaneously as the 1st still, and former standby still R3 switches as the 2nd still;
6) so move in circles, realize that the continuous countercurrent that simulates of ketene absorbs.
Described reactor cylinder inboard wall is equipped with longitudinal baffle, installs common stirring rake blade A1 on the stir shaft of described closed curved leaf disc turbine oar additional, has strengthened the gas dispersion effect, helps reaction to carry out rapidly and uniformly.For effectively controlling the temperature of reaction system, kettle barrel is equipped with chuck.Absorb fully by above cyclic ethylene ketone, the reaction solution production concentration that obtains reaches 83%.Reactor quantity is the 3-6 platform, realizes many stills cascade reaction.
The present invention has adopted closed curved leaf disc turbine oar to provide power for transfer of gas, make ketene under the low pressure condition, to realize to reactor from the cracking operation, and the conveying between the reactor, in actual production, if connecting, 2 stills fail to absorb fully ketene, can increase reactor series connection progression, and to not influence of transfer of gas; Common blade A1, closed curved leaf disc turbine oar A2, baffle plate A3 with the cylindrical shell inboard, ketene is mixed with acetone fully, and the reaction efficiency height is particularly for the absorption reaction of ketene in the 2nd grade and the later reactor, ketene content reduces step by step, but because acetone content improves step by step, effectively guaranteed the efficient absorption of ketene, reaction system approaches the continuous countercurrent reaction process; After the reaction of the 1st still was finished, the production concentration height can reach 80% even higher, and did not worry the problem that absorbs fully of follow-up ketene, and this has reduced cost for the separation of reaction solution.The simulation continuous countercurrent of having realized ketene absorbs.
Claims (7)
1. process for simulative continuous counter-current absorption of ketene by acetone, it is characterized by: 3 reactors are set at least, add reaction mass acetone and catalyzer in the described reactor, adopt 2 still cascade reactions, 1 still is awaited orders, 3 stills take turns blocked operation and absorb flow process, the reactor stirring rake adopts closed curved leaf disc turbine oar, and negative pressure realizes that the simulation continuous countercurrent of ketene absorbs, and the back level of described reactor is equipped with condenser and gas-liquid separator, the gas phase that produces in the reactor reaction process, through condenser condenses, gas-liquid separator separates, the described reactor of liquid-phase reflux, gas phase enters the next stage reactor, absorbs back tail gas and sends into the flare system processing.
2. according to the described a kind of process for simulative continuous counter-current absorption of ketene by acetone of claim 1, it is characterized in that:
1) ketene is delivered to the 1st still that series connection absorbs by the cracking operation, regulate the 1st still rotating speed of agitator, produce the negative pressure of 0～40kPa, suck ketene, under sufficient stirring and catalyst action, reaction heat is emitted in the ketene rapid reaction simultaneously, along with reaction is carried out, acetone steam and a small amount of unreacted ketene gas rise, through condenser condenses and gas-liquid separator separates, liquid phase is returned the 1st still, and gas phase enters the 2nd still;
2) the 2nd still reaction of series connection absorption is regulated the 2nd still rotating speed of agitator with the 1st still, produces the negative pressure of 0～40kPa, suck the remaining ketene gas in the 1st still reaction back, consider that the ketene gas concentration that enters is very low, reaction heat is less, suitably improves the needed temperature of reaction; Acetone steam and a spot of non-condensable gases are through condenser condenses and gas-liquid separator separates, and liquid phase is returned the 2nd still, the gas phase gas processing system that truncates;
3) standby still is got acetone and catalyzer ready, keeps suitable temperature, can cut at any time, as reactor;
4) the 1st still reacts to production concentration and reaches institute when requiring concentration, cuts out as standby still, emit reaction solution after, get the raw materials ready again, add acetone and catalyzer, keep suitable temperature;
5) when the 1st still cuts out as standby still, the 2nd still switches simultaneously as the 1st still, and former standby still switches as the 2nd still;
6) so move in circles, realize the continuous absorption of ketene.
3. according to claim 1 or 2 described a kind of process for simulative continuous counter-current absorption of ketene by acetone, it is characterized in that: described reactor cylinder inboard wall is equipped with longitudinal baffle, and the reactor cylindrical shell outside is equipped with chuck.
4. according to the described a kind of process for simulative continuous counter-current absorption of ketene by acetone of claim 1, it is characterized in that: be equipped with the stirring rake blade on the stir shaft of described closed curved leaf disc turbine oar.
5. according to the described a kind of process for simulative continuous counter-current absorption of ketene by acetone of claim 1, it is characterized in that: described reactor quantity is the 3-6 platform, realizes many stills cascade reaction.
6. according to the described a kind of process for simulative continuous counter-current absorption of ketene by acetone of claim 1, it is characterized in that: after described standby still adds acetone and catalyzer, pre-hot reserve, preheating temperature is 30～60 ℃.
7. according to the described a kind of process for simulative continuous counter-current absorption of ketene by acetone of claim 1, it is characterized in that: described reactor control reaction temperature is 40～100 ℃.
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| CN 200810204711 CN101747163B (en) | 2008-12-16 | 2008-12-16 | Process for simulative continuous counter-current absorption of ketene by acetone |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103342681A (en) * | 2013-05-31 | 2013-10-09 | 黄冈银河阿迪药业有限公司 | Process and device for improving utilization rate of ethylene oxide of metronidazole production raw materials |
| CN104373811A (en) * | 2013-08-14 | 2015-02-25 | 上海聚鼎半导体设备有限公司 | Homogeny gas conveying system |
| CN108854918A (en) * | 2018-08-14 | 2018-11-23 | 四川深蓝环保科技有限公司 | A kind of chemico-heating wash reaction system of waste mineral oil and the waste containing mineral oil |
| CN110170280A (en) * | 2019-05-14 | 2019-08-27 | 浙江恒澜科技有限公司 | The preparation method of high-temperature pyrolysis reactor and Pintsch process reaction system and ketene compounds |
| CN110511142A (en) * | 2019-08-29 | 2019-11-29 | 青岛科技大学 | A kind of continuous production system and production technology of methylvinyl acetate |
| CN114105748A (en) * | 2020-08-28 | 2022-03-01 | 万华化学集团股份有限公司 | Preparation method, prepared ketene compound and application of compound |
| CN116099455A (en) * | 2023-04-12 | 2023-05-12 | 西南化工研究设计院有限公司 | Carbonylation reaction system and method based on multi-kettle serial connection |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342681A (en) * | 2013-05-31 | 2013-10-09 | 黄冈银河阿迪药业有限公司 | Process and device for improving utilization rate of ethylene oxide of metronidazole production raw materials |
| CN104373811A (en) * | 2013-08-14 | 2015-02-25 | 上海聚鼎半导体设备有限公司 | Homogeny gas conveying system |
| CN108854918A (en) * | 2018-08-14 | 2018-11-23 | 四川深蓝环保科技有限公司 | A kind of chemico-heating wash reaction system of waste mineral oil and the waste containing mineral oil |
| CN110170280A (en) * | 2019-05-14 | 2019-08-27 | 浙江恒澜科技有限公司 | The preparation method of high-temperature pyrolysis reactor and Pintsch process reaction system and ketene compounds |
| CN110170280B (en) * | 2019-05-14 | 2022-09-02 | 浙江恒逸石化研究院有限公司 | High-temperature cracking reactor, high-temperature cracking reaction system and preparation method of ketene compounds |
| CN110511142A (en) * | 2019-08-29 | 2019-11-29 | 青岛科技大学 | A kind of continuous production system and production technology of methylvinyl acetate |
| CN114105748A (en) * | 2020-08-28 | 2022-03-01 | 万华化学集团股份有限公司 | Preparation method, prepared ketene compound and application of compound |
| CN116099455A (en) * | 2023-04-12 | 2023-05-12 | 西南化工研究设计院有限公司 | Carbonylation reaction system and method based on multi-kettle serial connection |
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