CN205253138U

CN205253138U - Cyclohexanone oxime ization reaction inactivation catalyst abluent device of unloading on line

Info

Publication number: CN205253138U
Application number: CN201520894385.0U
Authority: CN
Inventors: 李万清; 周学军; 李军; 游华彬; 车小军; 万军; 陈超
Original assignee: Hubei Sanning Chemical Co Ltd
Current assignee: Hubei Sanning Chemical Co Ltd
Priority date: 2015-11-09
Filing date: 2015-11-09
Publication date: 2016-05-25
Anticipated expiration: 2025-11-09

Abstract

The utility model provides a catalyst of the cyclohexanone oxime ization reaction belt cleaning device of unloading on line, catalyst blowpit bottom is connected through conveying pipeline line and delivery pump, catalyst blowpit top is connected through conveying pipeline line and circulative cooling ware, the conveying pipeline line of delivery pump closes back and filter sub -unit connection with the conveying pipeline congruence of circulative cooling ware, the filter bottom is connected through conveying pipeline line and subsider, filter upper portion is connected through conveying pipeline line and clear solution groove, clear solution tank bottom portion delivers to oximate reation kettle again after conveying pipeline and clear solution delivery pump are connected. Its method is that the turbid liquid of catalyst that draws off of oximate reation kettle moves back to the catalyst blowpit in, by the delivery pump from circulative cooling cooling back, carry again and clean and filtrate in the filter, filter catalyst thick liquid after the wasing subsider sedimentation that stews that directly impresses. The utility model discloses washes, washes and concentrated can the washing catalyst that contains reaction material that draws off in the reation kettle through mellow wine, materiel recovered, draw off the catalyst in organic matter content all be less than 500PPM.

Description

The device that the online discharging of a kind of cyclohexanone oximate reaction decaying catalyst is cleaned

Technical field

The cyclohexanone oximate catalysts that the utility model relates to unloads material cleaning device online, belongs to chemical process and apparatus field.

Background technology

Cyclohexanone oxime is to produce caprolactam important intermediate, is made by azanol and cyclohexanone generation oximation reaction. At present, the main production method of cyclohexanone oxime is, under the existence of titanium-silicon molecular sieve catalyst and t-butanol solvent, utilize hydrogen peroxide, ammonia and cyclohexanone reaction to generate cyclohexanone oxime, by built-in membrane filtration system, filtering molecular sieve catalyst, obtains reacting clear liquid, then obtains highly purified cyclohexanone oxime through a series of rectifying extraction process.

From the ruuning situation of current domestic amidoxime gasifying device, because catalyst exists certain coking deactivation and the situation of loss, in oximation reaction still, titanium-silicon molecular sieve catalyst need constantly add, to ensure the concentration of active catalyst. And accumulate in reactor because of the catalyst of coking deactivation, catalyst concn constantly rises, and causes built-in membrane filtration system filtration flux variation; On the other hand, although there be filling into of fresh catalyst, cause fresh catalyst to be coated and to affect its catalytic efficiency by decaying catalyst because decaying catalyst amount in reactor is excessive. Therefore, reactor needs irregular shut-down that decaying catalyst is all exited, and again drops into fresh catalyst and goes into operation. The work of stopping reactor expends a large amount of manpower and materials, has also affected the macrocyclic operation of efficient stable of amidoxime metallization processes.

Utility model CN201596496U, CN201988375U etc. relate to the Ammoximation reaction device of producing cyclohexanone oxime and report, but do not narrate for the processing of catalyst in production process. Therefore seek a kind of method by the online processing of catalyst and ensure that the operation of Ammoximation reaction device efficient stable necessitates.

Summary of the invention

The purpose of this utility model is to provide a kind of catalyst of cyclohexanone oximate reaction to unload online material cleaning device, for adapting to supplementing of cyclohexanone oxamidinating method technique.

The catalyst that the utility model provides unloads online material cleaning device and comprises catalyst blowpit, and is connected with catalyst filter through catalyst blowpit bottom by catalyst slurry delivery pump; Catalyst slurry delivery pump self-loopa pipeline is provided with cooler; Catalyst filter bottom is connected with catalyst sedimentation groove; Catalyst filter top is connected with clear liquid groove.

Described catalyst blowpit is with stirring, and gas phase is provided with drain and is connected with system, for the ammonia flashing off is reclaimed.

Described is provided with cooler on catalyst slurry delivery pump self-loopa pipeline, and cooling medium is recirculated water.

Described is connected on pipeline with catalyst filter at catalyst slurry delivery pump, is provided with the tert-butyl alcohol, demineralized water, N₂Pipeline, is respectively used to alcohol wash, washing and concentrated.

In described catalyst filter, be provided with metal filtering core, filter core quantity 50-100 root, filtering accuracy 0.3～1 μ m.

Described catalyst sedimentation groove is that a specification is long 10m, wide 6m, the stainless steel tank of high 1m.

Described catalyst filter upper clear supernate goes out stockline and is provided with demineralized water recoil pipeline, for preventing film blockage.

The described tert-butyl alcohol, demineralized water, N₂On pipeline and demineralized water recoil pipeline, be equipped with control valve and flowmeter, the DCS during for online discharging controls.

The utility model also provides a kind of online discharging cleaning method of catalyst of cyclohexanone oximate reaction, comprise the steps: that the turbid liquid of catalyst that oximation reaction still draws off retreats in catalyst blowpit, after the cooling cooling of delivery pump self-loopa, be delivered in filter again and carry out cleaning and filtering, the catalyst slurry filtering after cleaning is directly pressed into the separation of subsider standing sedimentation; The clear liquid filtering out is returned oximation reaction still by clear liquid delivery pump and is recycled after being collected by clear liquid groove.

Catalyst slurry first through tert-butyl alcohol washing, is removed cyclohexanone oxime in filter; Through demineralized water washing, remove the tert-butyl alcohol and ammonia again; Washing in filter, passes into N later₂, the water in a part of catalyst slurry is removed in pressurization.

The main component of catalyst slurry is catalyst 3～4%wt, ammonia 2～3%wt, tert-butyl alcohol 40-45%wt, water 30-35%, cyclohexanone oxime 15～20%wt; Main component through alcohol wash, washing, concentrated catalyst slurry is later catalyst 15～20%wt, water 85～80%.

The catalyst of a kind of cyclohexanone oximate reaction that the utility model provides unloads material cleaning device online, and its advantage is,

1, utilize the online discharging of catalyst, ensured the concentration of fresh catalyst in reactor, ensured preferably reaction effect.

2, use after this device, reactor does not need to stop and processes catalyst, has ensured reactor long-period stable operation.

3, the alcohol wash of this device setting, washing and the concentrated catalyst containing reaction mass drawing off in reactor can cleaning, material reclaims, and draws off in catalyst content of organics all lower than 500PPM.

Brief description of the drawings

Fig. 1 is that the catalyst of cyclohexanone oximate reaction unloads material cleaning device schematic diagram online, wherein, and 1. catalyst blowpit, 2. delivery pump, 3. recirculation cooler, 4. filter, 5. subsider, 6. clear liquid groove, 7. clear liquid delivery pump, the 8. turbid liquid carrier pipe of catalyst, 9. tert-butyl alcohol carrier pipe, 10. demineralized water carrier pipe, 11.N₂Carrier pipe, 13. demineralized water recoil pipelines.

Fig. 2 is the equipment schematic diagram of catalyst filter, wherein, and 12. filter cores.

Detailed description of the invention

Embodiment 1

As shown in Figure 1, a kind of catalyst of cyclohexanone oximate reaction unloads material cleaning device online, catalyst blowpit 1 bottom is connected with delivery pump 2 through conveying pipeline, catalyst blowpit 1 top is connected with recirculation cooler 3 through conveying pipeline, the conveying pipeline of delivery pump 2 closes afterwards and is connected with filter 4 bottoms with the conveying pipeline congruence of recirculation cooler 3, filter 4 bottoms are connected with subsider 5 through conveying pipeline, filter 4 tops are connected with clear liquid groove 6 through conveying pipeline, on this conveying pipeline, be also provided with demineralized water recoil pipeline 13, oximation reaction still is delivered in clear liquid groove 6 bottoms after conveying pipeline is connected with clear liquid delivery pump 7 again.

On conveying pipeline after the conveying pipeline of described delivery pump 2 and the conveying pipeline congruence of recirculation cooler 3 are closed, be also provided with tert-butyl alcohol carrier pipe 9, demineralized water carrier pipe 10 and N₂Carrier pipe 11.

In described filter 4, be also provided with filter core 12, this filter core 12 is metal powder sintered filter element, filter core quantity 50-100 root, filtering accuracy 0.3～1 μ m.

As shown in Figure 2, the equipment schematic diagram of filter 4, wherein built-in 80 metal sintering film pipes, film pipe filter core aperture is 0.3-1 μ m.

Embodiment 2

The utility model process implementing process is: the turbid liquid of catalyst that oximation reaction still draws off retreats in catalyst blowpit, after the cooling cooling of delivery pump self-loopa, then is delivered to and in filter, carries out cleaning and filtering. Filter cleaning step and be divided into alcohol wash, washing, concentrated three steps, respectively:

1, alcohol wash: the tert-butyl alcohol is introduced in catalyst filter to flow-control 0.5-3m³/ h, 1-3h post analysis is crossed cyclohexanone oxime content < 0.05% in cleaner liquid, and alcohol wash is qualified;

2, washing: demineralized water is introduced in catalyst filter to flow-control 1-5m³/ h, 1-3h post analysis is crossed t butanol content < 0.05% in cleaner liquid, and it is qualified to wash;

3, concentrated: by N₂In introducing catalyst filter, flow-control 1-3m³/ h, finishes concentrated after 10-30min.

Catalyst slurry after cleaning after filtration is directly pressed into catalyst sedimentation groove standing sedimentation and separates; The clear liquid filtering out is returned oximation reaction still by clear liquid delivery pump and is recycled after being collected by clear liquid groove.

Claims

1. the device that the online discharging of a cyclohexanone oximate reaction decaying catalyst is cleaned, it is characterized in that, catalyst blowpit (1) bottom is connected with delivery pump (2) through conveying pipeline, catalyst blowpit (1) top is connected with recirculation cooler (3) through conveying pipeline, the conveying pipeline of delivery pump (2) closes afterwards and is connected with filter (4) bottom with the conveying pipeline congruence of recirculation cooler (3), filter (4) bottom is connected with subsider (5) through conveying pipeline, filter (4) top is connected with clear liquid groove (6) through conveying pipeline, on this conveying pipeline, be also provided with demineralized water recoil pipeline (13), oximation reaction still is delivered in clear liquid groove (6) bottom after conveying pipeline is connected with clear liquid delivery pump (7) again.

2. the device that the online discharging of cyclohexanone oximate reaction decaying catalyst according to claim 1 is cleaned, it is characterized in that, on the conveying pipeline after the conveying pipeline congruence of the conveying pipeline of delivery pump (2) and recirculation cooler (3) is closed, be also provided with tert-butyl alcohol carrier pipe (9), demineralized water carrier pipe (10) and N₂Carrier pipe (11).

3. the device that the online discharging of cyclohexanone oximate reaction decaying catalyst according to claim 1 is cleaned, it is characterized in that, in filter (4), be also provided with filter core (12), this filter core (12) is metal powder sintered filter element, filter core quantity 50-100 root, filtering accuracy 0.3 ~ 1 μ m.