CN202778430U - Catalytic reaction separating device with internal and external combined films - Google Patents
Catalytic reaction separating device with internal and external combined films Download PDFInfo
- Publication number
- CN202778430U CN202778430U CN 201220142049 CN201220142049U CN202778430U CN 202778430 U CN202778430 U CN 202778430U CN 201220142049 CN201220142049 CN 201220142049 CN 201220142049 U CN201220142049 U CN 201220142049U CN 202778430 U CN202778430 U CN 202778430U
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- external
- catalytic reaction
- metal film
- pipeline
- retort
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- Expired - Lifetime
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- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims description 40
- 239000000919 ceramic Substances 0.000 claims description 19
- 238000003860 storage Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 3
- 238000009295 crossflow filtration Methods 0.000 claims description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 abstract description 22
- 239000003054 catalyst Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 238000000926 separation method Methods 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000007423 decrease Effects 0.000 abstract 2
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 16
- 239000000047 product Substances 0.000 description 15
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 10
- SFZULDYEOVSIKM-UHFFFAOYSA-N chembl321317 Chemical compound C1=CC(C(=N)NO)=CC=C1C1=CC=C(C=2C=CC(=CC=2)C(=N)NO)O1 SFZULDYEOVSIKM-UHFFFAOYSA-N 0.000 description 7
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000004087 circulation Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 230000001839 systemic circulation Effects 0.000 description 2
- 238000006237 Beckmann rearrangement reaction Methods 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 150000002443 hydroxylamines Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000006146 oximation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The utility model discloses a catalytic reaction separating device with internal and external combined films. The catalytic reaction separating device comprises a reaction tank, a dead end filtering device with an internal metal film, a cross flow filtering device with an external inorganic film, and a product storing tank, wherein the dead end filtering device with the internal metal film is arranged along the inner sidewall of the reaction tank; the large cycle of some materials is carried out between the reaction tank and the cross flow filtering device with the external inorganic film, and the small cycle of some materials is carried out in a closed circuit which is formed by the cross flow filtering device with the external inorganic film, a circulating pump and a small circulating pipeline; catalysts entering the cross flow filtering device with the external inorganic film are intercepted and then flow back into the reaction tank through a circulating pipeline; and catalysts in the reaction tank are intercepted by the dead end filtering device with the internal metal film. The catalytic reaction separating device with the internal and external combined films is specifically suitable for a cyclohexanone ammoximation process and a catalyst separation process of the ammoximation process. According to the catalytic reaction separating device, the size of an ammoximation tank is reduced, the filtering area of the dead end filtering device with the internal metal film is reduced, the amount of filter elements decreases, the investment on equipment is reduced, the energy consumption decreases, the continuity in separation of the catalysts is ensured, and the cycle of run is long.
Description
Technical field
The utility model relates to a kind of interior external combined films catalytic reaction separator, is applicable to cyclohexanone oxamidinating reaction and catalyst separation process thereof, also is applicable to other catalytic reaction and catalyst separation process thereof.
Technical background
Cyclohexanone oxime is a kind of important intermediate of producing caprolactam, is made by hydroxylamine salt and cyclohexanone generation oximation reaction, and the cyclohexanone oxime of generation obtains caprolactam through Beckmann rearrangement again.At present, the method for preparing cyclohexanone oxime mainly contains Raschig process (HSO), NO catalytic reduction method (NO method), phosphatic hydroxylamine method (HPO), cyclohexanone oxamidinating method (HAO).The sulphur ammonium of HSO method, NO method complex process and by-product low value wherein; Although the 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.Have the problem that the amidoxime method has overcome above-mentioned three aspects: only, the preparation method is simple, and by-product sulphur ammonium without an environmental protection difficult problem, therefore quite is not subjected to the favor of caprolactam industry in recent years.
The standby cyclohexanone oxime of amidoxime legal system is at first by the invention of Italian ENI company, and at first set up in Italy and produce 10000 tons amidoxime experimental rig per year, built up in Japan in 2003 and produce 60000 tons amidoxime chemical industry device per year, the domestic amidoxime chemical industry device of producing 70000 tons per year and producing 100000 tons per year that also built up respectively.
From the present domestic amidoxime chemical industry device ruuning situation of building up, all there are some problems.Adopt single external ceramic membrane systemic circulation filter, then behind the Ammoximation reaction, product need be transported to carries out separating of cyclohexanone oxime and catalyst in the filter, and filter needs regular on-line regeneration and irregular regenerated offline, and the cycle of operation is short; Simultaneously, for guaranteeing the tangent line linear speed of filter, reactor material self-loopa amount is larger, has increased energy consumption.Because catalyst interception rate is had relatively high expectations, the filter area of filter is larger, and the filter apparatus investment is larger.Adopt single built-in metal film dead-end filtration, then constantly increase at the cartridge surface filter cake thickness, transmembrane pressure also increases thereupon, and filtration resistance increases, and the penetrating power of filtrate reduces.In order to guarantee the penetrating power of filtrate, then the filter area of metal film increases, and filter core quantity increases, and reactor volume increases, and can affect the conversion ratio of cyclohexanone, and simultaneously equipment investment also can increase.And in ZL201120054873.2, adopt built-in filter and external filter to filter step by step, and then the built-in filter filter area is large, and filter core quantity is many, and the retort volume is large, and equipment investment is high.This shows, at present the drawbacks such as cyclohexanone oxamidinating catalysts separation equipment cost of investment height, separation process energy consumption height.
In sum, for solving all difficult problems in the caprolactam production process cyclohexanone oxamidinating operation, energy savings reduces production costs, and the cyclohexanone oxamidinating reaction separating device is improved, and is to reduce caprolactam production cost urgent problem.
The utility model content
The utility model is for the deficiency of existing cyclohexanone oxamidinating catalysts separation process technique, cyclohexanone oxamidinating reactor and catalyst separation process thereof are improved, the interior external combined films catalytic reaction separator that a kind of energy consumption is low, cost is low is provided.
For achieving the above object, the utility model adopts following technical scheme:
A kind of interior external combined films catalytic reaction separator, the built-in metal film dead-end filtration device, external inoranic membrane cross-flow filter and the product storage tank that comprise retort, arrange along the madial wall of described retort; Described retort bottom is provided with raw material feed distributor and reacting product outlet, and the top is provided with the recycle stock distributor; Described external inoranic membrane cross-flow filter comprises feeding pipeline, inorganic membrane assembly and the recycle stock pipeline with charging pump, the two ends of described feeding pipeline connect respectively the reacting product outlet of described retort bottom and the entrance of inorganic membrane assembly, and the two ends of described recycle stock pipeline connect respectively the dope outlet of described inorganic membrane assembly and the recycle stock distributor at described retort top; The purified liquor outlet of the built-in metal film dead-end filtration device in the described retort and the purified liquor outlet of external inoranic membrane cross-flow filter are connected with described product storage tank through pipeline respectively.
Described raw material feed distributor and recycle stock distributor are the endless tube that evenly has distribution hole.
Be communicated with by the partial circulating material pipe between the feeding pipeline of described external inoranic membrane cross-flow filter and the recycle stock pipeline, and feeding pipeline is provided with circulating pump near described inorganic membrane assembly arrival end.
The film pore of described built-in metal film dead-end filtration device and inorganic membrane assembly directly is 0.05～10 μ m.
Described inorganic membrane assembly is two groups, and two groups are connected in parallel between described feeding pipeline and the recycle stock pipeline.
The inoranic membrane of described inorganic membrane assembly is ceramic membrane or metal film.
The technological progress that the utility model is obtained:
1, owing to adopts the catalytic reaction separator of built-in metal film cross-flow filter and external inoranic membrane cross-flow filter synchronous filtering, alleviated the filter pressure of built-in filter in single built-in film filter filter type and the interior external filter substep filter type, reduced the filter area of built-in filter, reduced the quantity of built-in filter filter core, the volume that has reduced retort is controlled in the zone of reasonableness retort volume, has reduced the equipment investment of built-in filter and retort; Reduced the operation energy consumption of single external ceramic membrane systemic circulation filter.
2, because external inoranic membrane cross-flow filter adopts the cross-flow filtration mode of partial circulating, reduce the circulation pump lift, reduced operation energy consumption.
3, because inorganic membrane assembly adopts two groups, adopt one group filtering during operation, the mode that another group is used in the switching of cleaning and regeneration, the disruption of catalyst separation when having solved inorganic membrane assembly regeneration, guaranteed the continuity of catalyst separation, made the device cycle of operation long.
Description of drawings
Fig. 1 is the utility model structural representation.
Fig. 2 is the structural representation of retort of the present utility model.
Fig. 3 is the top view of retort internal structure.
In the accompanying drawings: 1 recycle stock pipeline, 2 retort, 3 built-in metal film dead-end filtration devices, 4 charging pumps, 5 circulating pumps, 6 ceramic film components, the purified liquor outlet of 7 external inoranic membrane cross-flow filters, 8 product storage tanks, the purified liquor outlet of 9 built-in metal film dead-end filtration devices, 10 raw material feed distributors, 11 reacting product outlets, 12 agitators, 13 recycle stock distributors, 14 feeding pipelines, 15 partial circulating material pipes.
The specific embodiment
Embodiment 1
Such as Fig. 1, Fig. 2, shown in Figure 3, built-in metal film dead-end filtration device 3, external inoranic membrane cross-flow filter and product storage tank 8 that present embodiment comprises retort 2, arranges along the madial wall of described retort 2; Described external inoranic membrane cross-flow filter comprises feeding pipeline 14, ceramic film component 6 and the recycle stock pipeline 1 with charging pump 4, the two ends of described feeding pipeline connect respectively the reacting product outlet 11 of described retort 2 bottoms and the entrance of ceramic film component 6, and the two ends of described recycle stock pipeline 1 connect respectively the dope outlet of described ceramic film component 6 and the recycle stock distributor 13 at described retort 2 tops; The purified liquor outlet 9 of described built-in metal film dead-end filtration device 3 and the purified liquor outlet 7 of external inoranic membrane cross-flow filter are connected with described product storage tank 8 through pipeline respectively.
As shown in Figure 2, described raw material feed distributor 10 and recycle stock distributor 13 are the endless tube that evenly has distribution hole.
Be communicated with by partial circulating material pipe 15 between the feeding pipeline 14 of described external inoranic membrane cross-flow filter and the recycle stock pipeline 1, and feeding pipeline 14 is provided with circulating pump 5 near described ceramic film component 6 arrival ends.
The film pore of described built-in metal film dead-end filtration device 3 and ceramic film component 6 directly is 0.05～10 μ m.
Described ceramic film component 6 is two groups, and two groups are connected in parallel between described feeding pipeline 14 and the recycle stock pipeline 1.
Present embodiment is used for the technical process that cyclohexanone amidoxime catalytic reaction separates: reaction raw materials, solvent tertiary butanol and catalyst from retort 2 bottoms in raw material feed distributor 10 enters retort 2, a reacted product part directly is that the built-in metal film dead-end filtration device 3 of 0.05～10 μ m filters through the film pores in the retort 2, and it directly is that the ceramic film component 6 of 0.05～10 μ m carries out synchronous filtering that another part enters into the film pore from the reacting product outlet 11 of retort 2 bottoms.The catalyst dope of being held back by external ceramic film component 6 enters in the retort 2 through recycle stock pipeline 1 and recycle stock distributor 13, under agitator 12 effects, carry out Ammoximation reaction, stay retort 2 interior sustainable participation catalytic reactions through the suspended state catalyst that built-in metal film dead-end filtration device 3 is held back, the clear liquid that the clear liquid that sees through through built-in metal film dead-end filtration device 3 and external ceramic membrane cross-flow filter see through links to each other with cyclohexanone oxime product storage tank 8 with 7 through purified liquor outlet 9 respectively.
Ceramic film component 6 is two groups in the present embodiment, and when wherein one group when filtering, another is organized at cleaning and regeneration.So repeatedly carry out.
External inoranic membrane cross-flow filter is the partial circulating filtered version, most reaction mass is back in the retort 2 through recycle stock pipeline 1 and recycle stock distributor 13 through another part reaction mass dope that ceramic film component 6 is held back in the closed circuit high speed circulation that feeding pipeline 14, circulating pump 5, ceramic film component 6, partial circulating material pipe 15 etc. form; In partial circulating, cyclohexanone oxime clear liquid permeation ceramic membrane enters into product cyclohexanone oxime product storage tank 8 through purified liquor outlet 7.
Replace ceramic film component 6 with metal film in the present embodiment, other are with embodiment 1.
The utility model also can be used for other catalytic reactions and catalyst separation process thereof.
Claims (6)
1. external combined films catalytic reaction separator in a kind, the built-in metal film dead-end filtration device (3), external inoranic membrane cross-flow filter and the clear liquid storage tank (8) that it is characterized in that comprising retort (2), arrange along the madial wall of described retort (2); Described retort (2) bottom is provided with raw material feed distributor (10) and reacting product outlet (11), and the top is provided with recycle stock distributor (13); Described external inoranic membrane cross-flow filter comprises feeding pipeline (14), inorganic membrane assembly (6) and the recycle stock pipeline (1) with charging pump (4), the two ends of described feeding pipeline connect respectively the reacting product outlet (11) of described retort (2) bottom and the entrance of inorganic membrane assembly (6), and the two ends of described recycle stock pipeline (1) connect respectively the dope outlet of described inorganic membrane assembly (6) and the recycle stock distributor (13) at described retort (2) top; The purified liquor outlet (9) of the built-in metal film dead-end filtration device in the described retort (2) and the purified liquor outlet (7) of external inoranic membrane cross-flow filter are connected with described product storage tank (8) through pipeline respectively.
2. interior external combined films catalytic reaction separator according to claim 1 is characterized in that described raw material feed distributor (10) and recycle stock distributor (13) are the endless tube that evenly has distribution hole.
3. interior external combined films catalytic reaction separator according to claim 1, it is characterized in that being communicated with by partial circulating material pipe (15) between the feeding pipeline (14) of described external inoranic membrane cross-flow filtration device and the recycle stock pipeline (1), and feeding pipeline (14) is provided with circulating pump (5) near described inorganic membrane assembly (6) arrival end.
4. interior external combined films catalytic reaction separator according to claim 1 is characterized in that the film pore of described built-in metal film dead-end filtration device (3) and inorganic membrane assembly (6) directly is 0.05～10 μ m.
5. interior external combined films catalytic reaction separator according to claim 1 is characterized in that described inorganic membrane assembly (6) is two groups, and two groups are connected in parallel between described feeding pipeline (14) and the recycle stock pipeline (1).
6. interior external combined films catalytic reaction separator according to claim 1, the inoranic membrane that it is characterized in that described inorganic membrane assembly (6) is ceramic membrane or metal film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220142049 CN202778430U (en) | 2012-04-06 | 2012-04-06 | Catalytic reaction separating device with internal and external combined films |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220142049 CN202778430U (en) | 2012-04-06 | 2012-04-06 | Catalytic reaction separating device with internal and external combined films |
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| Publication Number | Publication Date |
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| CN202778430U true CN202778430U (en) | 2013-03-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201220142049 Expired - Lifetime CN202778430U (en) | 2012-04-06 | 2012-04-06 | Catalytic reaction separating device with internal and external combined films |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262196A (en) * | 2014-09-02 | 2015-01-07 | 河北美邦工程科技有限公司 | Ammoximation reaction and separation coupling process and device |
| CN107362756A (en) * | 2017-09-06 | 2017-11-21 | 钦州聚力新能源科技有限公司 | Using the petrochemical production equipment and production technology of cross-flow filter |
| CN110743367A (en) * | 2019-10-28 | 2020-02-04 | 南京工业大学 | Automatic filtering system and process |
| CN112426957A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Heterogeneous ammoximation reaction separation device 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 |
-
2012
- 2012-04-06 CN CN 201220142049 patent/CN202778430U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262196A (en) * | 2014-09-02 | 2015-01-07 | 河北美邦工程科技有限公司 | Ammoximation reaction and separation coupling process and device |
| CN107362756A (en) * | 2017-09-06 | 2017-11-21 | 钦州聚力新能源科技有限公司 | Using the petrochemical production equipment and production technology of cross-flow filter |
| CN110743367A (en) * | 2019-10-28 | 2020-02-04 | 南京工业大学 | Automatic filtering system and process |
| CN110743367B (en) * | 2019-10-28 | 2022-10-14 | 南京工业大学 | Automatic filtering system and process |
| CN112426957A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Heterogeneous ammoximation reaction separation device 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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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 12, building 050035, 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 construction hi tech A-17L, No. 9 Changjiang Road, Hebei, Shijiazhuang Patentee before: Hebei Meibang Engineering Technology Co., Ltd. |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130313 |