CN202700369U - Dynamic separation device for cyclohexanone ammoximation catalysts - Google Patents
Dynamic separation device for cyclohexanone ammoximation catalysts Download PDFInfo
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- CN202700369U CN202700369U CN 201220294588 CN201220294588U CN202700369U CN 202700369 U CN202700369 U CN 202700369U CN 201220294588 CN201220294588 CN 201220294588 CN 201220294588 U CN201220294588 U CN 201220294588U CN 202700369 U CN202700369 U CN 202700369U
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Abstract
The utility model relates to a dynamic separation device for cyclohexanone ammoximation catalysts. The dynamic separation device comprises a charging pump and dynamic separators, wherein a charging end pipeline of the charging pump is connected with a reaction still, a discharging end pipeline of the charging pump is communicated with at least one dynamic separator, suspension liquid outlet end pipelines of dynamic separators returns back to the upper portion of the reaction still, and clear liquid outlet end pipelines of dynamic separators are connected with a clear liquid collector. By the aid of the dynamic separation device, the safety problems of membrane tube damage, acid-base consumption, wastewater discharge and membrane tube replacement which are caused by periodic cleaning of membrane component plugs are creatively solved, simultaneously, a reaction liquid external circulation system is not required, catalyst abrasion and energy consumption increase which are caused by the external circulation system are reduced, shutdown caused by replacement of membrane components is avoided, cleaning and consumption costs of membrane tubes are saved, and the production requirements are met.
Description
Technical field
The utility model relates to a kind of cyclohexanone oxamidinating catalyst Dynamic Separation device, is a kind of method of cyclohexanone oxamidinating catalyst Dynamic Separation specifically.
Background technology
At present, the commercial run of producing in the world caprolactam take cyclohexanone oxime as intermediate has the techniques such as phosphatic hydroxylamine method, HAS method, PNC process for caprolactam and cyclohexanone oxamidinating method, it is a kind of brand-new technique that the cyclohexanone oxamidinating method is produced caprolactam, Italy's ENI is developed and industrialization the earliest, in recent years, domestic also develop the amidoxime metallization processes.This technique has that technological process is short, energy consumption is low, operating condition is gentle and the advantage such as environmental protection, produce needed main raw material(s) and comprise cyclohexanone, hydrogen peroxide, liquefied ammonia and titanium-silicon molecular sieve catalyst, reaction dissolvent is the tert-butyl alcohol, product is cyclohexanone oxime, there is gas-liquid-solid three-phase in reaction system, reactor is with interior agitator, simultaneously for guaranteeing that three-phase is uniformly dispersed and prevents catalyst sedimentation, sticking wall.In technological design, designed outside the reactor and forced systemic circulation by mechanical pump, titanium-silicon molecular sieve catalyst and reacted solution carry out isolated by filtration in ceramic film component, under the effect of operation pressure reduction, solution less than membrane aperture is sent to rear operation by ceramic membrane, catalyst is then cut on the mould surface and by regularly face being carried out back flush, makes catalyst come back to reaction system.The traditional ceramics film separation system comprises two parts, be that external circulating system and the ceramic film component that pump and reactor form filters and backwashing system, membrane module adopts many groups " string also " formula structure, namely form group by the membrane module series winding, then group again and be unified into large group, the assembly of large group carries out " up and down " intermittent filtration or recoil simultaneously.When actual production is filtered, the upper membrane module filtration pressure difference of every group film is larger than lower membrane module, upper membrane module filtration yield is also large than lower membrane module, because ceramic membrane surface is often because of easily blocked or pollution of a variety of causes, the upper membrane module that filtration yield is large degree blocked or that pollute is more serious, and when recoil, stop up or upper membrane module that pollution level is more serious because of the not following membrane module of the high repercussion effect of pressure reduction, so vicious circle, guaranteeing in the constant situation of total filtration yield, then cause the membrane module filter capacity to descend first, increase lower membrane module load, and then cause lower membrane module filter capacity to descend, final so that all film inlet outlet pressure differentials, transmembrane pressure rises, affect total filtration flux and production capacity, cause load down or parking.Membrane module after the pollution need to carry out the soda acid Chemical cleaning, every group of membrane module cleaning charge is about about 50,000 yuan, annual cleaning total cost will reach 5,000,000 yuan, and waste a large amount of soda acids and fresh water (FW) and produce 30,000 tons of waste water because cleaning, and the annual electricity consumption of outer circulation will reach 1,600,000 degree.Therefore, we stopped because changing membrane module in the urgent need to a kind of both having avoided, and had saved again cleaning and the consumption costs of film pipe, had satisfied the cyclohexanone oxamidinating catalyst Dynamic Separation device of the needs of producing.
Summary of the invention
In view of above-mentioned technical deficiency, the purpose of this utility model is to provide a kind of cyclohexanone oxamidinating catalyst Dynamic Separation device, this cyclohexanone oxamidinating catalyst Dynamic Separation device has been simplified the catalyst separation flow process, reduced because ceramic membrane stops up and cleaned the series of malpractice of bringing, reduce investment outlay, energy savings and effectively reduce operating cost, have great economic benefit and social benefit.
The technical solution of the utility model is: a kind of cyclohexanone oxamidinating catalyst Dynamic Separation device, feed pump and dynamic separator have been comprised, the feed end pipeline of described feed pump is connected with reactor, the discharge end pipeline of described feed pump leads to the dynamic separator of at least one, the turbid liquid outlet end pipeline of described dynamic separator is back to the middle and upper part of reactor, and the clear liquid outlet end pipeline of described dynamic separator is connected with the clear liquid collector.
In one embodiment, described dynamic separator comprises tank body, described tank body top is provided with material inlet, described tank body lower part is provided with turbid liquid outlet and purified liquor outlet, be equipped with a rotating shaft in the described tank body, the video disc film filtering element is installed in the described rotating shaft, described rotating shaft is by the motor-driven that is arranged on the tank body top, described motor is regulated its rotating speed of control by frequency converter, in order to control video disc film filtering element rotary speed and liquid crossflow velocity.
In one embodiment, described video disc film skin covering of the surface surface current speed control is built in 0～20m/s.
In one embodiment, this device also comprises a can,douche, and described can,douche top is connected with pressure charging system, and the flushing line of described can,douche bottom is connected on the clear liquid outlet end pipeline, in order to inputting clear liquid and back flush video disc film filtering element to can,douche.
In one embodiment, the described frequency of oppositely rushing is 0 ~ 20 time/10 minutes.
The beneficial effects of the utility model are as follows:
The one, adopt Dynamic Membrane to separate and substitute the separation of traditional ceramics film, be about to pass through built-in video disc film filtering element with the turbid liquid of catalyst and reactant mixture, isolate clear liquid, the band catalyst mixed liquid then is intercepted at the film surface and by timing face is carried out back flush, make catalyst get back to reaction system, video disc film skin covering of the surface surface current speed control is built in 0～20m/s, and the recoil frequency is 0 ~ 20 time/10 minutes.
Two is that 100,000 ton/years of amidoxime process units of a cover dispose 16 groups of ceramic film component needs (large membrane module quantity is converted according to filtration yield) routinely, membrane module inlet outlet pressure differential often occurs because film pollutes and the transmembrane pressure height needs cleaning during shutdown membrane module or integral replacing film pipe, 16 annual replacings of membrane module are cleaned by 80 calculating, change 1200 of film pipes, the each cleaning needs 200 tons of water, 2.5 ton nitric acid, 2.5 ton caustic soda, about 30000 yuan, change one group of membrane module and need 50,000 yuan, change 1200 yuan of film pipes, total cost 5,000,000; Dynamic separator video disc film filtering element of the present invention can stop up the face problem by fine solution catalyst, can clean separator online separately, and cleaning liquid measure only is 1/10th of former ceramic film component, and the waste water total amount only is 1/20th, cleans the frequency and is no more than annual 30 times.Cleaning total cost can be controlled in 500,000 yuan.The present invention has simplified the catalyst separation flow process, has reduced because ceramic membrane stop up to clean the series of malpractice of bringing, and reduces investment outlay, energy savings and effectively reduce operating cost.Have great economic benefit and social benefit.
The 3rd, it is a kind of brand-new technique that the cyclohexanone oxamidinating method is produced caprolactam, it has that technological process is short, energy consumption is low, operating condition is gentle and the advantage such as environmental protection, this technique has competitiveness and development prospect in all preparing process of caprolactam, and membrane filtration system is the key point of this technique successful Application, adopt Dynamic Membrane to separate substituting the separation of traditional ceramics film is a completely new concept, have than former mode and to be unsurpassed in excellence, the dynamic membrane filtering system is applicable nm-class catalyst and the reactant liquor separation system of being similar to too.
Description of drawings
Fig. 1 is the syndeton schematic diagram of the cyclohexanone oxamidinating catalyst Dynamic Separation device in implementing.
Description of drawings: 1-feed pump, 2-dynamic separator, 3-feed end pipeline, the 4-reactor, 5-discharge end pipe, 6-clear liquid outlet end pipeline, 7-clear liquid collector, 8-material inlet, the turbid liquid outlet of 9-, the 10-purified liquor outlet, 11-rotating shaft, 12-video disc film filtering element, the 13-motor-driven, the turbid liquid outlet end of 14-pipeline, 15-can,douche, the 16-frequency converter, 17-pressure charging system, 18-flushing line.
The specific embodiment
For above-mentioned feature and advantage of the present utility model can be become apparent, embodiment cited below particularly, and cooperation accompanying drawing be described in detail below, but the utility model are not limited to this.
With reference to legend 1, a kind of cyclohexanone oxamidinating catalyst Dynamic Separation device, feed pump 1 and dynamic separator 2 have been comprised, the feed end pipeline 3 of described feed pump 1 is connected with reactor 4, the discharge end pipeline 5 of described feed pump 1 leads to the dynamic separator 2 of at least one, the turbid liquid outlet end pipeline 14 of described dynamic separator 2 is back to the middle and upper part of reactor 4, and the clear liquid outlet end pipeline 6 of described dynamic separator 2 is connected with clear liquid collector 7.Above-mentioned structure is cyclohexanone oxamidinating catalyst Dynamic Separation circulating pipe system.
In the present embodiment, described dynamic separator comprises tank body, described tank body top is provided with material inlet 8, described tank body lower part is provided with turbid liquid outlet 9 and purified liquor outlet 10, be equipped with a rotating shaft 11 in the described tank body, in the described rotating shaft 11 video disc film filtering element 12 be installed, described rotating shaft 11 is driven by the motor 13 that is arranged on the tank body top, described motor 13 is regulated its rotating speed of control by frequency converter 16, in order to control video disc film filtering element rotary speed and liquid crossflow velocity.
In the present embodiment, described video disc film skin covering of the surface surface current speed control is built in 0～20m/s.
In the present embodiment, this device also comprises a can,douche 15, described can,douche 15 tops are connected with pressure charging system 17, and the flushing line 18 of described can,douche 15 bottoms is connected on clear liquid outlet end 6 pipelines, in order to inputting clear liquid and back flush video disc film filtering element to can,douche.
In the present embodiment, the described frequency of oppositely rushing is 0 ~ 20 time/10 minutes.
The Dynamic Separation method is that the turbid liquid with catalyst and reactant mixture is passed through built-in video disc film filtering element, under the effect of pressure reduction, seeing through the disc-type membrane component less than the solution of membrane aperture enters the clear liquid collector and goes rear operation, then flow with relative crossflow velocity at membrane surface with catalyst mixed liquid, catalyst is intercepted at the film surface and by regularly face being carried out back flush, makes catalyst get back to reaction system.One independently the Dynamic Membrane piece-rate system formed by two parts, be feed pump and dynamic separator, in design, can select as required one or more groups dynamic separator parallel operation, feed pump can share also and can dispose separately, dynamic separator is one and is with built-in diaphragm and rotatable equipment, adjusting rotary speed is to satisfy certain crossflow velocity needs as required for rotating speed, and each group dynamic separator can arrange interval backflushing to clean the film surface, realizes long-term operation.Cross send into after cleaner liquid filters through the secondary security after system to reclaim solvent, simplified the catalyst separation flow process, reduced because ceramic membrane stops up and cleaned the series of malpractice of bringing, reduce investment outlay, energy savings and effectively reduce operating cost.
The above only is preferred embodiment of the present utility model, and all equalizations of doing according to the utility model claim change and modify, and all should belong to covering scope of the present utility model.
Claims (5)
1. cyclohexanone oxamidinating catalyst Dynamic Separation device, feed pump and dynamic separator have been comprised, it is characterized in that: the feed end pipeline of described feed pump is connected with reactor, the discharge end pipeline of described feed pump leads to the dynamic separator of at least one, the turbid liquid outlet end pipeline of described dynamic separator is back to the middle and upper part of reactor, and the clear liquid outlet end pipeline of described dynamic separator is connected with the clear liquid collector.
2. cyclohexanone oxamidinating catalyst Dynamic Separation device according to claim 1, it is characterized in that: described dynamic separator comprises tank body, described tank body top is provided with material inlet, described tank body lower part is provided with turbid liquid outlet and purified liquor outlet, be equipped with a rotating shaft in the described tank body, the video disc film filtering element is installed in the described rotating shaft, described rotating shaft is by the motor-driven that is arranged on the tank body top, described motor is regulated its rotating speed of control by frequency converter, in order to control video disc film filtering element rotary speed and liquid crossflow velocity.
3. cyclohexanone oxamidinating catalyst Dynamic Separation device according to claim 2, it is characterized in that: described video disc film skin covering of the surface surface current speed control is built in 0～20m/s.
4. cyclohexanone oxamidinating catalyst Dynamic Separation device according to claim 1, it is characterized in that: this device also comprises a can,douche, described can,douche top is connected with pressure charging system, the flushing line of described can,douche bottom is connected on the clear liquid outlet end pipeline, in order to inputting clear liquid and back flush video disc film filtering element to can,douche.
5. cyclohexanone oxamidinating catalyst Dynamic Separation device according to claim 4, it is characterized in that: the described frequency of oppositely rushing is 0 ~ 20 time/10 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220294588 CN202700369U (en) | 2012-06-21 | 2012-06-21 | Dynamic separation device for cyclohexanone ammoximation catalysts |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220294588 CN202700369U (en) | 2012-06-21 | 2012-06-21 | Dynamic separation device for cyclohexanone ammoximation catalysts |
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| CN202700369U true CN202700369U (en) | 2013-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201220294588 Expired - Lifetime CN202700369U (en) | 2012-06-21 | 2012-06-21 | Dynamic separation device for cyclohexanone ammoximation catalysts |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114643024A (en) * | 2021-12-07 | 2022-06-21 | 上海安赐环保科技股份有限公司 | Industrialized device and process for liquid-phase thermal synthesis of lithium iron phosphate |
| CN114984621A (en) * | 2022-07-19 | 2022-09-02 | 福建永荣科技有限公司 | Equipment for settling and separating catalyst in ammoximation reaction |
-
2012
- 2012-06-21 CN CN 201220294588 patent/CN202700369U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114643024A (en) * | 2021-12-07 | 2022-06-21 | 上海安赐环保科技股份有限公司 | Industrialized device and process for liquid-phase thermal synthesis of lithium iron phosphate |
| CN114643024B (en) * | 2021-12-07 | 2024-03-22 | 上海安赐环保科技股份有限公司 | Industrial device and process for lithium iron phosphate liquid-phase thermal synthesis |
| CN114984621A (en) * | 2022-07-19 | 2022-09-02 | 福建永荣科技有限公司 | Equipment for settling and separating catalyst in ammoximation reaction |
| CN114984621B (en) * | 2022-07-19 | 2023-06-16 | 福建永荣科技有限公司 | Catalyst sedimentation separation equipment for ammoximation reaction |
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| C14 | Grant of patent or utility model | ||
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| TR01 | Transfer of patent right |
Effective date of registration: 20170414 Address after: Shimen Ao Dong Zhuang Industrial Park town of Xiuyu District 351156 Fujian city of Putian Province Patentee after: FUJIAN EVERSUN TECHNOLOGY Co.,Ltd. Address before: 350206 Fujian city of Fuzhou province Changle City Airport Industrial Zone Pengcheng Road No. 28 Patentee before: Fujian Jinjiang Petrochemical Co.,Ltd. |
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Granted publication date: 20130130 |
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| CX01 | Expiry of patent term |