CN203816603U - Ammoximation reaction system for preparing cyclohexanone oxime - Google Patents

Ammoximation reaction system for preparing cyclohexanone oxime Download PDF

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Publication number
CN203816603U
CN203816603U CN201320708186.7U CN201320708186U CN203816603U CN 203816603 U CN203816603 U CN 203816603U CN 201320708186 U CN201320708186 U CN 201320708186U CN 203816603 U CN203816603 U CN 203816603U
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China
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tank body
outlet
inlet
pipeline
filter
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CN201320708186.7U
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Chinese (zh)
Inventor
张电子
李磊
郑晓广
李识寒
王大勇
景国耀
禹保卫
余保银
杜卫民
孙超伟
任文杰
庞向川
张恒超
窦晓勇
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Nylon Science And Technology Ltd Of China Ping Meishen Horse Group
SHENMA INDUSTRIAL Co Ltd
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Nylon Science And Technology Ltd Of China Ping Meishen Horse Group
SHENMA INDUSTRIAL Co Ltd
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Priority to CN201320708186.7U priority Critical patent/CN203816603U/en
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Abstract

The utility model discloses an ammoximation reaction system for preparing cyclohexanone oxime. The ammoximation reaction system comprises a reaction device, an external circulating device and an external filtering device, wherein the reaction device is provided with an external circulating outlet, an external circulating inlet, a tank body clear liquid discharging hole and a catalyst inlet, the external circulating outlet is connected with the inlet of the external circulating device through a pipeline, and the outlet of the external circulating device is connected with the external circulating inlet; the tank body clear liquid discharging hole is connected with the inlet of the external filtering device through a pipeline, and the outlet of the external filtering device is connected with the inlet of the external circulating device through a pipeline. According to the ammoximation reaction system, by arranging a flow guiding cylinder and a baffle in a tank body, after reaction materials enter the flow guiding cylinder at the upper part of a stirrer in the tank body through a mixer and baffled by virtue of the baffle, catalysts freely settle. The ammoximation reaction system has the beneficial effects that a filter system in a tank can be omitted, the external filtering load and the backwashing frequency are reduced, the life of the system is prolonged, and the load of the reactor is reduced.

Description

A kind of Ammoximation reaction system for the preparation of cyclohexanone oxime
Technical field
The utility model relates to a kind of Ammoximation reaction system, relates in particular to a kind of Ammoximation reaction system for the preparation of cyclohexanone oxime, belongs to chemical technology field.
Background technology
Cyclohexanone oxime is the important intermediate of preparing caprolactam.The method of preparing in the world at present cyclohexanone oxime mainly contains HAS method (HSO method), nitric oxide reduction method (NO method), phosphatic hydroxylamine method (HPO method) and amidoxime method (HAO method).The sulphur ammonium of HSO method and NO method complex process and by-product low value wherein; Although HPO method is by-product sulphur ammonium not, technical process requires meticulous, and operation easier is large, and has NOx to produce, and has the difficult problem of environmental protection.At present, cyclohexanone oxime mainly utilizes cyclohexanone to prepare by Ammoximation reaction, has the problem that amidoxime method has overcome above-mentioned several respects only.Amidoxime legal system for cyclohexanone oxime method simply, not by-product sulphur ammonium, without the difficult problem of environmental protection, therefore be quite subject in recent years the favor of caprolactam industry.
The amidoxime legal system of cyclohexanone oxime is proposed by Italian ENI company the earliest for cyclohexanone oxime.So far successively in Japan and China, built up nearly 10 cover commercial plants, total productive capacity approaches 1,000,000 tons.From the current domestic amidoxime chemical industry device ruuning situation of building up, all there are some problems.After Ammoximation reaction, product need be transported to carries out the separated of cyclohexanone oxime and catalyst in filter, and filter needs regularly recoil regeneration; Because Ammoximation reaction is exothermic reaction, reaction heat can not make full use of, and causes very large waste in separation process.As can be seen here, at present Ammoximation reaction separation equipment has the drawbacks such as separation process complexity, utilization of Heat of Reaction are unreasonable.
Existing catalyst separation device is built-in, and because Ammoximation reaction is exothermic reaction, in course of reaction, obvious rising may appear in temperature, thereby makes reaction temperature wayward under optimal reaction temperature and affect reaction speed.After Ammoximation reaction completes, directly in reactor, product is carried out separated with solid catalyst.Yet built-in catalyst separation device easily stops up in separation process, therefore need to stop production and clean and keep in repair completely, not only treatment cycle is longer, and numerous and diverse and dangerous.For another example, clear liquid and catalyst separation system after Ammoximation reaction, no matter be reactor inner filtration, outer filtration or inside and outside dual filtration system, filter all needs high frequency recoil regeneration, the processing load of reactor and filtration system is large, the time between overhauls(TBO) of reactor and filter is short, causes start-stop product frequency high.
In sum, a difficult problem for catalyst separation, saves the energy and reduces costs when solving amidoxime legal system for cyclohexanone oxime, and amidoxime chemical industry gasifying device is improved, and is to reduce amidoxime to change into this, promote amidoximeization and produce load urgent problem.
Utility model content
For the existing deficiency of prior art, technical problem to be solved in the utility model is to provide a kind of Ammoximation reaction system for the preparation of cyclohexanone oxime.This system overhaul cycle is long, and it is low that amidoxime changes into.
For realizing above-mentioned utility model object, the utility model provides following reaction unit:
For the preparation of an Ammoximation reaction device for cyclohexanone oxime, described reaction unit comprises tank body, agitator;
Described tank interior is also provided with guide shell, and described guide shell is on described agitator top, and described guide shell is connected in and described tank body center by support.
Described tank inner surface is also provided with baffle plate, and described baffle plate is perpendicular to described tank inner surface.
Wherein more preferably, described tank body internal diameter is 1.5:1~2.5:1 with the ratio of described guide shell internal diameter.
Wherein more preferably, described tank body internal diameter is 2:1 with the ratio of described guide shell internal diameter.
Wherein more preferably, described baffle plate is 1/8~1/9 of described tank body internal diameter away from one side of described tank inner surface and the distance of described guide shell outer surface.
Wherein more preferably, described guide shell bottom is 60~70% of described tank body height apart from the distance of described tank base.
Wherein more preferably, described tank body clear liquid discharging opening is positioned at described tank body middle and upper part, apart from tank base distance, is 55~65% of described tank body height; Outer circulation outlet is positioned at described tank body middle and upper part, apart from tank base distance, is 70~75% of described tank body height.
The utility model adopts following technical proposals:
For the preparation of an Ammoximation reaction system for cyclohexanone oxime, comprise reaction unit, external circulating device, outer filter;
Described reaction unit is provided with outer circulation outlet, outer circulation entrance, tank body clear liquid discharging opening and catalyst inlet;
Described outer circulation outlet is connected with the entrance of described external circulating device by pipeline, and the outlet of described external circulating device is connected with described outer circulation entrance by pipeline;
Described tank body clear liquid discharging opening is connected with the entrance of described outer filter by pipeline, and the outlet of described outer filter is connected with the entrance of described external circulating device by pipeline.
Wherein more preferably, described reaction unit comprises the agitator in tank body and built-in described tank body, and described tank body is offered outer circulation outlet, outer circulation entrance, tank body clear liquid discharging opening, catalyst inlet.
Wherein more preferably, described tank interior is also provided with guide shell, and described guide shell is on described agitator top, and described guide shell is connected by support and described tank body.
Wherein more preferably, described tank inner surface is also provided with baffle plate, and described baffle plate is perpendicular to described tank inner surface.
Wherein more preferably, described reaction unit is also provided with nitrogen inlet and gaseous phase outlet.
Wherein more preferably, described external circulating device comprises heat exchanger, feed(raw material)inlet, blender, described outer circulation outlet is connected with described heat exchanger entrance by pipeline, described heat exchanger exit, feed(raw material)inlet are connected by pipeline with described mixer entrance respectively, and described mixer outlet is connected with described outer circulation entrance by pipeline.
Wherein more preferably, described outer filter comprises that filter, described filter offer recoil entrance, the filter outlet of filter inlet, purified liquor outlet, regeneration;
Described tank body clear liquid discharging opening is connected with described filter inlet by pipeline, and described filter outlet links by pipeline and described feed(raw material)inlet.
Cyclohexanone oxime Ammoximation reaction system provided by the utility model, makes system save tank inner filtration system by guide shell and baffle plate are set, and has reduced outer filtration load and recoil frequency extension device life-span, reduces reactor load.
Accompanying drawing explanation
Fig. 1 is the utility model cyclohexanone oxime Ammoximation reaction system architecture schematic diagram.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
As shown in Figure 1, the utility model provides a kind of Ammoximation reaction system for the preparation of cyclohexanone oxime (hereinafter to be referred as cyclohexanone oxime Ammoximation reaction system), comprises reaction unit 1, external circulating device 2, outer filter 3; Reaction unit 1 is provided with outer circulation outlet 12, outer circulation entrance 14, tank body clear liquid discharging opening 15 and catalyst inlet 18; Outer circulation outlet 12 is connected with the entrance of external circulating device 2 by pipeline, and the outlet of external circulating device 2 is connected with outer circulation entrance 14 by pipeline; Tank body clear liquid discharging opening 15 is connected with the entrance of outer filter 3 by pipeline, and the outlet of outer filter 3 is connected with the entrance of external circulating device 2 by pipeline.Below the utility model cyclohexanone oxime Ammoximation reaction system is launched to describe in detail.
As shown in Figure 1, reaction unit 1 comprises the agitator 11 in tank body 10 and built-in tank body 10, on agitator 11, blade is installed, and blade is by driven by motor.Tank body 10 is offered outer circulation outlet 12, outer circulation entrance 14, tank body clear liquid discharging opening 15, catalyst inlet 18.Tank body clear liquid discharging opening 15 is positioned at tank body 10 middle and upper parts, apart from tank body 10 distances from bottom, is preferably 55~65% of tank body 10 height; Outer circulation outlet 12 is positioned at tank body 10 middle and upper parts, apart from tank body 10 distances from bottom, is preferably 70~75% of tank body height.The tert-butyl alcohol containing finite concentration catalyst enters reaction unit 1 by catalyst inlet 18, the reaction heat of reaction unit 1 shifts out reaction unit 1 by circulating pump by outer circulation outlet 12, through heat exchanger 21, utilize heat exchanger 21 to take away, reactant liquor enters reaction unit 1 together with reaction mass by outer circulation entrance 14.In order to maintain the pressure balance of reaction unit 1, tank body 10 is also provided with nitrogen inlet 16 and gaseous phase outlet 17.
As shown in Figure 1, in order to guarantee that reaction mass moves upward in tank body 10 under the effect of agitator 11 and fully to mix generation chemical reaction, and make to react clear liquid with catalyst sedimentation with separated, in tank body 10 inside, be also provided with guide shell 13, guide shell 13 is arranged on agitator 11 tops.Guide shell 13 upper/lower terminal openings.Preferably guide shell internal diameter is 1.5:1~2.5:1 with tank body internal diameter ratio.Preferably guide shell 13 bottoms are 60~70% of described tank body 10 height apart from the distance of tank body 10 bottoms.Between guide shell 13 outer surfaces and tank body 10 inner surfaces, have for reacting the passage that clear liquid flows through.Reaction mass enters guide shell 13 and from guide shell 13 bottoms, along guide shell 13 inner surfaces, moves upward under the effect of agitator 11, and through liquid level baffling, the passage between guide shell 13 outer guide shell 13 outer surfaces and tank body 10 inner surfaces moves downward reaction mass.
As shown in Figure 1, for further making the inner surface that reacts clear liquid described tank body 10 separated with catalyst sedimentation also be provided with baffle plate 19, baffle plate 19 is perpendicular to tank body 10 inner surfaces.Preferably in the passage of baffle plate 19 between guide shell 13 outer surfaces and tank body 10 inner surfaces.Preferably baffle plate is 1/8~1/9 of tank body internal diameter away from one side of tank inner surface and the distance of guide shell outer surface.Reaction mass forms baffling district at baffle plate 19 places.Reaction mass moves downward after baffle plate 19 places stop liquid level baffling outside guide shell 13, in guide shell 13 bottoms, is divided into two parts, and a part is returned guide shell 13, and a part is gone back to the baffling district of baffle plate 19.The baffling district that reaction mass forms at baffle plate 19 places remains static substantially, reaction clear liquid and catalyst carry out sedimentation separation at this, the overflow of upper strata reaction clear liquid enters filter 3 by tank body clear liquid discharging opening 15, the catalyst of lower floor again enters guide shell 13 under the effect of agitator 11, and so forth circulation.
As shown in Figure 1, external circulating device 2 comprises heat exchanger 21, feed(raw material)inlet 22, blender 23, outer circulation outlet 12 is connected with the entrance of heat exchanger 21 by pipeline, the outlet of heat exchanger 21, feed(raw material)inlet 22 are connected by pipeline with the entrance of blender 23 respectively, and the outlet of blender 23 is connected with outer circulation entrance 14 by pipeline.The reaction heat of reaction system is shifted out by outer circulation outlet 12 by circulating pump, through heat exchanger 21, takes away reaction heat, and the reactant liquor shifting out with reaction heat enters blender 23.Ammonia, hydrogen peroxide, cyclohexanone are blended in t-butanol solvent and enter blender 23 by feed(raw material)inlet 22, through the mixed reactant liquor of blender 23, together with reaction mass, by outer circulation entrance 14, enter guide shell 13.
As shown in Figure 1, described outer filter 3 comprises filter 30, purified liquor outlet 31, recoil entrance 32; Tank body clear liquid discharging opening 15 is connected with the entrance of filter 30 by pipeline, and the outlet of filter 30 is connected with feed(raw material)inlet 22 by pipeline.Reaction clear liquid is from 15 outflows of tank body clear liquid discharging opening after filter 30 filters, and filtrate is returned to external circulating device 2 by pipeline, so circulation.
The reaction unit 1 of take below with guide shell 13 and baffle plate 19 is preference with external circulating device 2, the common cyclohexanone oxime Ammoximation reaction system forming of outer filter 3, and the course of work of the utility model Ammoximation reaction system is launched to describe in detail.
3 assemblings of the reaction unit 1 that the utility model provides, external circulating device 2, outer filter start cyclohexanone oxime Ammoximation reaction system after joining and finishing.Reaction mass gas ammonia, hydrogen peroxide, cyclohexanone, the tert-butyl alcohol enter blender 23 by feed(raw material)inlet 22, after blender 23 mixes, by outer circulation entrance 14, enter guide shell 13.Controlling nitrogen inlet 16 and gaseous phase outlet 17 adjusts the pressure of reaction unit 1 (preferably 0.2Mpa~0.3Mpa), adjusts the external environmental factors such as the suitable amidoxime method of temperature reaction that heat exchanger 21 makes reaction unit 1.The tert-butyl alcohol containing finite concentration catalyst (TS-1 molecular sieve) enters reaction unit by catalyst inlet 18.Reaction conversion ratio and selective better when catalyst concn is greater than the interior mean value (preferably 0.5% left and right) of reactor.Reaction mass enters after the guide shell 13 in tank body 10, mixes and the abundant chemical reaction that occurs under the effect of agitator 11.Reaction mass moves upward along guide shell 13 inner surfaces from guide shell 13 bottoms under the effect of agitator 11, and through liquid level baffling, the passage between guide shell 13 outer guide shell 13 outer surfaces and tank body 10 inner surfaces moves downward reaction mass.Reaction mass moves downward after baffle plate 19 places stop liquid level baffling outside guide shell 13, in guide shell 13 bottoms, is divided into two parts, and a part is returned guide shell 13, and a part is gone back to the baffling district of baffle plate 19.Reaction mass remains static substantially in baffle plate 19 baffling districts, reaction clear liquid and catalyst carry out preliminary sedimentation separation at this, the overflow of upper strata reaction clear liquid enters filter 3 by tank body clear liquid discharging opening 15, the catalyst of lower floor again enters guide shell under the effect of agitator 11, and so forth circulation.Reaction clear liquid in upper strata, containing the catalyst of low concentration, enters filter 30 from tank body clear liquid discharging opening 15 flows out.After filter 30 filters, clear liquid is discharged by purified liquor outlet 31; Filtrate is discharged by filter outlet, and in this filtrate, catalyst concn is higher.Filtrate is returned to external circulating device 2 by pipeline, and so forth circulation.Reactant liquor shifts out reaction unit 1 by circulating pump by outer circulation outlet 12, and through heat exchanger 21, the reactant liquor after heat exchanger 21 heat exchange enters blender 23 to be mixed, and reactant liquor enters guide shell 13 together with reaction mass by outer circulation entrance 14, and so forth circulation.
By this cyclohexanone oxime Ammoximation reaction system, reaction clear liquid in reaction mass and catalyst are in baffle plate 19 places sedimentation separation, 70~80% catalyst is separated, in reaction clear liquid, catalyst content accounts for 0.5~0.8%, the load of filter 30 significantly decline (catalyst concn drops to 0.5%~0.8% by 3%), recoil frequency, by recoil in original 2 minutes 1 time, reduces to recoil in 30~60 minutes 1 time, the service life of improving filter membrane.
In sum, the cyclohexanone oxime Ammoximation reaction system that the utility model provides has been saved tank inner filtration system, has reduced outer filtration load and recoil frequency.Having reduced catalyst runs off after filtration because of fragmentation.And then can reach the life-span that extends filter, reduce reactor load.
Above cyclohexanone oxime Ammoximation reaction system provided by the utility model is had been described in detail.For one of ordinary skill in the art, any apparent change of under the prerequisite that does not deviate from the utility model connotation, it being done, all will form the utility model infringement of patent right, will bear corresponding legal liabilities.

Claims (1)

1. for the preparation of an Ammoximation reaction system for cyclohexanone oxime, it is characterized in that, comprise reaction unit, external circulating device, outer filter;
Described reaction unit is provided with outer circulation outlet, outer circulation entrance, tank body clear liquid discharging opening and catalyst inlet;
Described outer circulation outlet is connected with the entrance of described external circulating device by pipeline, and the outlet of described external circulating device is connected with described outer circulation entrance;
Described tank body clear liquid discharging opening is connected with the entrance of described outer filter by pipeline, and the outlet of described outer filter is connected with the entrance of described external circulating device by pipeline.
2. Ammoximation reaction system as claimed in claim 1, is characterized in that, described reaction unit comprises tank body and be built in the agitator in described tank body, and described tank body is offered outer circulation outlet, outer circulation entrance, tank body clear liquid discharging opening, catalyst inlet.
3. Ammoximation reaction system as claimed in claim 2, is characterized in that, described tank inner surface is also provided with baffle plate, and described baffle plate is perpendicular to described tank body; Described tank interior is provided with guide shell, and described guide shell is positioned at described agitator top.
4. Ammoximation reaction system as claimed in claim 1, is characterized in that, described reaction unit is also provided with nitrogen inlet and gaseous phase outlet.
5. Ammoximation reaction system as claimed in claim 1, is characterized in that, described external circulating device comprises heat exchanger, feed(raw material)inlet, blender;
Described outer circulation outlet is connected with described heat exchanger entrance by pipeline, and described heat exchanger exit, feed(raw material)inlet are connected by pipeline with described mixer entrance respectively, and described mixer outlet is connected with described outer circulation entrance by pipeline.
6. Ammoximation reaction system as claimed in claim 5, is characterized in that,
Described outer filter comprises that filter, described filter offer recoil entrance, the filter outlet of filter inlet, purified liquor outlet, regeneration;
Described tank body clear liquid discharging opening is connected with described filter inlet by pipeline, and described filter outlet links by pipeline and described feed(raw material)inlet.
CN201320708186.7U 2013-11-08 2013-11-08 Ammoximation reaction system for preparing cyclohexanone oxime Expired - Lifetime CN203816603U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103551087A (en) * 2013-11-08 2014-02-05 神马实业股份有限公司 Ammoximation reaction system for preparing cyclohexanone-oxime
CN115212599A (en) * 2022-08-10 2022-10-21 聊城鲁西聚酰胺新材料科技有限公司 Material circulating system of cyclohexanone oxime rectifying tower reboiler

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103551087A (en) * 2013-11-08 2014-02-05 神马实业股份有限公司 Ammoximation reaction system for preparing cyclohexanone-oxime
CN103551087B (en) * 2013-11-08 2015-11-18 神马实业股份有限公司 A kind of Ammoximation reaction system for the preparation of cyclohexanone oxime
CN115212599A (en) * 2022-08-10 2022-10-21 聊城鲁西聚酰胺新材料科技有限公司 Material circulating system of cyclohexanone oxime rectifying tower reboiler

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Granted publication date: 20140910