CN204097374U - A kind of cyclohexanone oxamidinating reaction and tripping device - Google Patents
A kind of cyclohexanone oxamidinating reaction and tripping device Download PDFInfo
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- CN204097374U CN204097374U CN201420585816.0U CN201420585816U CN204097374U CN 204097374 U CN204097374 U CN 204097374U CN 201420585816 U CN201420585816 U CN 201420585816U CN 204097374 U CN204097374 U CN 204097374U
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Abstract
The utility model relates to the reaction of a kind of cyclohexanone oxamidinating and tripping device.Comprise reactor, reactor outer wall is provided with chuck or tube exchanger, material sparger, agitator, metal film filter is provided with in reactor, the material outlet of reactor bottom successively by pipeline and recycle pump, first-class heat exchanger, one-level feed in raw material mixing reactor or (with) feed in raw material mixing reactor, static mixer, secondary heat exchanger of secondary be connected, secondary heat exchanger is connected with recycle stock import by pipeline.Metal film filter is arranged with double-deck or individual layer membrane stack mode in reactor, and every layer has 1 ~ 10 group of membrane stack to be evenly distributed in reactor same plane, and in metal film filter, the filtering accuracy of metallic membrane is 0.05 ~ 5 μm.The utility model utilizes multi-form interchanger, achieves reaction heat recycling, improves cyclohexanone oxamidinating reaction and the efficiency be separated, avoids catalyst loss, reduce energy consumption and facility investment.
Description
Technical field
The utility model relates to a kind of chemical reaction equipment, and particularly a kind of cyclohexanone oxamidinating reaction and tripping device, belong to technical field of chemical engineering.
Background technology
As everyone knows, at chemistry, chemical technology field, hexanolactam is the main raw material producing nylon-6, and it is processed further can become polyamide fibre and engineering plastics.Cyclohexanone-oxime is the important source material of producing hexanolactam, and obtained by hydroxylammonium salt and pimelinketone generation oximation reaction, cyclohexanone-oxime obtains hexanolactam through Beckmann rearrangement again.At present, the method preparing cyclohexanone-oxime mainly contains Raschig process (HSO), NO catalytic reduction method (NO method), phosphatic hydroxylamine method (HPO), cyclohexanone oxamidinating method (HAO).Wherein HSO method, NO method complex process and the sulphur ammonium of by-product low value; Although HPO method is by-product sulphur ammonium not, technological process requires meticulous, and operation easier is large, and has NO
xproduce, there is the problem of contaminate environment.Oximes method overcomes the problem of above-mentioned three aspects, and preparation method is simple, and not by-product sulphur ammonium, non-environmental-pollution, therefore quite favors by industry in recent years.Cyclohexanone oxamidinating method is that means cyclohexanone is under the effect of TS-1 molecular sieve catalyst, react with the mixing solutions of hydrogen peroxide and ammonia and generate cyclohexanone-oxime, reaction product and solid catalyst is needed to draw outside reactor after having reacted, be separated through filter again, reaction product cyclohexanone-oxime clear liquid after filtration enters subsequent handling, is returned reactor continue to participate in catalyzed reaction by the catalyst transport that strainer retains.The deficiency that the method exists is, reaction feed liquid needs to be delivered to outside reactor, energy consumption is caused to increase, catalyzer is in course of conveying, because the shearing of pump makes catalyst abrasion, catalyst performance is caused to decline and loss, in order to solve the defect that traditional Ammoximation reaction and sepn process exist, energy efficient, reduce the loss of catalyzer, reduce production cost, present applicant has proposed a kind of new Ammoximation reaction and separating technology, for this reason, be necessary to improve existing Ammoximation reaction and tripping device.
Summary of the invention
The purpose of this utility model is to provide a kind of cyclohexanone oxamidinating to react and tripping device, for adapting to the improving technique of cyclohexanone oxamidinating method.
It is such that the utility model solves the scheme that its technical problem takes, a kind of cyclohexanone oxamidinating reaction and tripping device, comprise reactor, agitator is provided with in reactor, reactor internal upper part is provided with material sparger, in reactor, bottom is provided with metal film filter, metal film filter is arranged in same plane in membrane stack mode, reactor lower side is provided with reaction product cyclohexanone-oxime purified liquor outlet, Polycondensation Reactor and Esterification Reactor end is provided with recycle stock outlet, reactor top is provided with recycle stock import, catalyst inlet, reactor outer wall is provided with chuck or tube exchanger, the recycle stock outlet of Polycondensation Reactor and Esterification Reactor end connects recycle pump successively by pipeline, first-class heat exchanger, one-level is fed in raw material mixing reactor, static mixer, static mixer is connected with the recycle stock import at reactor top by pipeline.When adopt one-level feed in raw material mixing reactor time, one-level mixing reactor both sides of feeding in raw material respectively are provided with 2 charging openings, namely establish 4 charging openings altogether.
Above static mixer, establish secondary heat exchanger, size is opened in the reaction controlling situation adjustment according to cyclohexanone-oxime.
As optimization design, connect secondary and feed in raw material mixing reactor above one-level feeds in raw material mixing reactor, the secondary mixing reactor that feeds in raw material is connected with static mixer by pipeline.According to technological design, when adopt secondary feed in raw material mixing reactor time, one-level mixing reactor and the secondary mixing reactor that feeds in raw material that feeds in raw material respectively is provided with 2 charging openings, and charging opening can be located at the both sides of reinforced mixing reactor.Wherein, one-level feed in raw material mixing reactor charging opening in add ammonia and hydrogen peroxide respectively, or ammonia and pimelinketone, or ammonia and the trimethyl carbinol; The charging openings of two reinforced mixing reactors add pimelinketone and the trimethyl carbinol respectively, or the trimethyl carbinol and hydrogen peroxide, or pimelinketone and hydrogen peroxide.Pimelinketone and the trimethyl carbinol can be added respectively in mixing reactor, or the trimethyl carbinol and hydrogen peroxide otherwise one-level is fed in raw material, or pimelinketone and hydrogen peroxide.Ammonia and hydrogen peroxide can be added respectively, or ammonia and pimelinketone in the charging opening of two reinforced mixing reactors, or ammonia and the trimethyl carbinol.
Agitator adopts variable frequency regulating speed control rotating speed, and speed range is 0 ~ 150rpm.
Material sparger adopts circle shaped tube type, and pipeline has distribution hole.
Metal film filter in reactor can divide two-layer or mono-layer fashion layout, every layer has 1 ~ 10 group of membrane stack to be evenly distributed in same plane, membrane stack is supported fixing by the back up pad fixing with reactor inwall, each membrane stack is made up of several metallic membranes, the per-meate side of each metallic membrane forms clear liquid pipeline by pipe influx together, clear liquid pipeline is connected with the reaction product cyclohexanone-oxime purified liquor outlet of reactor lower side, and metal film filter filtering accuracy is 0.05 ~ 5 μm.
The beneficial effect that the utility model obtains is: adopt external charging hybrid reaction, raw material adds from the reinforced mixing reactor of reactor outside, make pimelinketone catalyzed reaction start to carry out in reactor outer circulation pipeline, add the reaction times, improve pimelinketone transformation efficiency.Adopt built-in metal film filter, improve catalyzed reaction and the efficiency be separated, avoid the leakage of catalyzer simultaneously, add security.Interchanger on chuck on reactor outer wall or external coiled pipe type interchanger and reactor external pipe achieves the recycling of reaction heat, reduces energy consumption and facility investment that Ammoximation reaction and catalyzer run.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Fig. 2 is that in reactor, metal film filter stacks vertical view.
Number in the figure implication is as follows:
1, reactor 2, chuck or tube exchanger 3, metal film filter 4, cyclohexanone-oxime purified liquor outlet 5, agitator 6, recycle stock outlet 7, recycle pump 8, interchanger 9, 11, one-level is fed in raw material mixing reactor charging opening 10, one-level is fed in raw material mixing reactor 13, secondary feeds in raw material mixing reactor 12, 14, secondary feeds in raw material mixing reactor charging opening 15, static mixer 16, secondary heat exchanger 17, recycle stock import 18, material sparger 19, catalyst inlet.
Embodiment
The specific embodiment provided below in conjunction with accompanying drawing and accompanying drawing is further described the utility model.
As shown in Figure 1, the reaction of the utility model cyclohexanone oxamidinating and tripping device, comprise reactor 1.Reactor 1 outer wall is provided with tube exchanger 2, is provided with agitator 5 in reactor 1, and adopt variable frequency regulating speed control rotating speed, speed range is 0 ~ 150rpm, and general rotating speed controls at about 130 rpm.Reactor 1 internal upper part is fixed with circle shaped tube type material sparger 18 by support, and circle shaped tube type material sparger pipeline has distribution hole, and vertical feed pipe lower end communicates with the circulating line of level.In reactor 1, bottom is provided with metal film filter 3.See figure, 2, metal film filter 3 is two-layer layout, every one deck to be evenly distributed in still in same plane by 6 groups of membrane stacks, metal film filter membrane stack is supported fixing by the back up pad fixing with reactor inwall, each membrane stack is made up of several metallic membranes, and the per-meate side of each metallic membrane forms clear liquid pipeline by pipe influx together, and clear liquid pipeline communicates with the reaction product cyclohexanone-oxime purified liquor outlet 4 of reactor 1 lower wall.Metal film filter 3 filtering accuracy is 0.05 ~ 5 μm, and market can be buied.Reactor 1 bottom is provided with recycle stock outlet 6, reactor top is provided with recycle stock import 17, catalyst inlet 19, the material outlet 6 of reactor 1 bottom connects recycle pump 7 successively by pipeline, first-class heat exchanger 8, one-level feed in raw material mixing reactor 10, secondary feeds in raw material mixing reactor 13, static mixer 15, secondary heat exchanger 16, secondary heat exchanger 16 is connected by the recycle stock import 17 of pipeline with reactor 1 top, feed pipe lower end and horizontal positioned circle shaped tube type sparger 18 communicate.One-level mixing reactor 10, the secondary mixing reactor 13 that feeds in raw material that feeds in raw material respectively is provided with 2 charging openings.Wherein, recycle pump, interchanger, static mixer, metal film filter etc. can be buied from market, are known features.
Principle of work of the present utility model is such: in reactor 1, add catalyzer TS-1 molecular sieve, ammonia, hydrogen peroxide, pimelinketone and the trimethyl carbinol, set up circulation, the pressure controlled in reactor 1 is 0.3 ~ 0.6Mpa, temperature is 75 ~ 95 DEG C, turn on agitator 5 and recycle pump 7, the rotating speed controlling agitator 5 is 0 ~ 150rpm, catalyzer TS-1 molecular sieve is added continuously in reactor 1, ammonia is added continuously in one-level feeds in raw material mixing reactor 10, hydrogen peroxide, secondary feeds in raw material in mixing reactor 13 and adds pimelinketone and the trimethyl carbinol continuously, to feed in raw material mixing reactor 10 in two-stage, 13 and static mixer 15 cyclohexanone carry out preliminary Ammoximation reaction, the first half in reactor 1, unreacted pimelinketone proceeds Ammoximation reaction, now the transformation efficiency of pimelinketone reaches more than 99.8%, obtain cyclohexanone-oxime solution.Lower Half in reactor 1, under pressure, cyclohexanone-oxime solution after filtration precision is that the metal film filter 3 of 0.05 ~ 5 μm is separated, cyclohexanone-oxime clear liquid oozes out into subsequent handling by exporting 4, catalyzer is trapped within reactor 1, via the recycle stock outlet 6 bottom reactor 1, recycle pump 7, first-class heat exchanger 8 enters two-stage and to feed in raw material mixing reactor 10, in 13, with the ammonia adding one-level continuously and feed in raw material in mixing reactor 10, feed in raw material pimelinketone in mixing reactor 13 and the trimethyl carbinol of hydrogen peroxide and secondary proceeds after catalyzed reaction through static mixer 15, secondary heat exchanger 16 and pipeline turn back in reactor 1 and realize circulating reaction and be separated, control interchanger 16 according to response situation and open size.Or one-level is fed in raw material in mixing reactor 10 and added pimelinketone, the trimethyl carbinol, secondary feeds in raw material in mixing reactor 13 and adds ammonia and hydrogen peroxide; Or one-level is fed in raw material in mixing reactor 10 and added ammonia, pimelinketone, secondary feeds in raw material in mixing reactor 13 and adds the trimethyl carbinol and hydrogen peroxide; Or one-level is fed in raw material in mixing reactor 10 and added the trimethyl carbinol and hydrogen peroxide, secondary feeds in raw material in mixing reactor 13 and adds ammonia, pimelinketone; Or one-level is fed in raw material in mixing reactor 10 and added ammonia, the trimethyl carbinol, secondary feeds in raw material in mixing reactor 13 and adds pimelinketone and hydrogen peroxide; Or one-level is fed in raw material in mixing reactor 10 and added pimelinketone and hydrogen peroxide, secondary feeds in raw material in mixing reactor 13 and adds ammonia, the trimethyl carbinol.
Claims (6)
1. a cyclohexanone oxamidinating reaction and tripping device, comprise reactor (1), reactor (1) outer wall is provided with chuck or tube exchanger (2), agitator (5) is provided with in reactor (1), reactor (1) internal upper part is fixed with material sparger (18) by support, it is characterized in that reactor (1) interior bottom is provided with metal film filter (3), metal film filter (3) is evenly distributed in same plane in membrane stack mode, metal film filter membrane stack is supported fixing by the back up pad fixing with reactor inwall, reactor (1) lower side is provided with reaction product cyclohexanone-oxime purified liquor outlet (4), Polycondensation Reactor and Esterification Reactor end is provided with recycle stock outlet (6), reactor top is provided with recycle stock import (17), catalyst inlet (19), recycle stock outlet (6) of reactor (1) bottom connects recycle pump (7) successively by pipeline, first-class heat exchanger (8), one-level is fed in raw material mixing reactor (10), static mixer (15), static mixer (15) is connected with the recycle stock import (17) at reactor (1) top by pipeline, one-level mixing reactor (10) both sides of feeding in raw material respectively are provided with 2 charging openings.
2. reaction according to claim 1 and tripping device, it is characterized in that being connected with secondary heat exchanger (16) in static mixer (15) top, secondary heat exchanger (16) is connected with the recycle stock import (17) at reactor (1) top by pipeline.
3. reaction according to claim 1 and 2 and tripping device, it is characterized in that being connected with secondary feeding in raw material mixing reactor (13) in one-level mixing reactor (10) top of feeding in raw material, the secondary mixing reactor (13) that feeds in raw material is connected by pipeline with static mixer (15), and one-level mixing reactor (10) and the secondary mixing reactor (13) that feeds in raw material that feeds in raw material respectively is provided with 2 charging openings.
4. reaction according to claim 1 and tripping device, is characterized in that agitator (5) is for variable frequency regulating speed control rotating speed, speed range 0 ~ 150rpm.
5. reaction according to claim 1 and tripping device, is characterized in that material sparger (18) is circle shaped tube type, circulating line has distribution hole.
6. reaction according to claim 1 and tripping device, it is characterized in that the metal film filter (3) in reactor (1) is two-layer or mono-layer fashion layout, every layer has 1 ~ 10 group of membrane stack, each membrane stack is made up of several metallic membranes, the per-meate side of each metallic membrane forms clear liquid pipeline by pipe influx together, and clear liquid pipeline is connected with the reaction product cyclohexanone-oxime purified liquor outlet of reactor lower side.
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| CN201420585816.0U CN204097374U (en) | 2014-10-11 | 2014-10-11 | A kind of cyclohexanone oxamidinating reaction and tripping device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174850A (en) * | 2019-10-11 | 2021-01-05 | 福建天辰耀隆新材料有限公司 | Cyclohexanone oxime preparation system and preparation method |
| CN112426958A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Ammoximation reaction separation device and method |
| WO2021208202A1 (en) * | 2020-04-13 | 2021-10-21 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced cyclohexanone ammoximation reaction system and method |
-
2014
- 2014-10-11 CN CN201420585816.0U patent/CN204097374U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174850A (en) * | 2019-10-11 | 2021-01-05 | 福建天辰耀隆新材料有限公司 | Cyclohexanone oxime preparation system and preparation method |
| WO2021208202A1 (en) * | 2020-04-13 | 2021-10-21 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced cyclohexanone ammoximation reaction system and method |
| CN112426958A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Ammoximation reaction separation device and method |
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Address after: 12, building 050000, Yee Yee building, 98 the Yellow River Avenue, Hebei, Shijiazhuang Patentee after: Hebei Mei Bang engineering science and technology limited-liability company Address before: 050035 Shijiazhuang Changjiang Road, Hebei, No. 9 building high-tech international A-17L Patentee before: Hebei Meibang Engineering Technology Co., Ltd. |