CN206253115U - A kind of heterogeneous catalytic reaction is combined the unit with UF membrane - Google Patents
A kind of heterogeneous catalytic reaction is combined the unit with UF membrane Download PDFInfo
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- CN206253115U CN206253115U CN201621285147.0U CN201621285147U CN206253115U CN 206253115 U CN206253115 U CN 206253115U CN 201621285147 U CN201621285147 U CN 201621285147U CN 206253115 U CN206253115 U CN 206253115U
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Abstract
The utility model is related to a kind of heterogeneous catalytic reaction to be combined the unit with UF membrane.Reaction upper end is provided with recycle stock import, catalyst charging hole and material inlet, retort bottom is provided with recycle stock outlet and liquefied ammonia import, retort lateral wall is provided with purified liquor outlet, metal film filter, guide shell, agitator, feed distributor and liquefied ammonia distributor are provided with retort, circulating pump is connected with charging mixer, heat exchanger, static mixer by pipeline on external circulation line, static mixer is connected with recycle stock import, and recycle stock outlet is connected with circulating pump.A circulating line is provided between circulating pump and charging mixer on external circulation line or is provided with external dead-end filter or is provided with external cross-flow filter.Suitable for cyclohexanone oxamidinating reactive separation process and other gas-liquid-solid three phase catalytic reaction separation processes such as diacetylmonoxime, expoxy propane, epoxychloropropane, hydrogen peroxide are prepared, production capacity is high, good effect of heat exchange, is easy to maintenance.
Description
Technical field
The utility model is related to a kind of chemical reaction equipment, and particularly a kind of heterogeneous catalytic reaction combines dress with UF membrane
Put, it is adaptable to cyclohexanone oxamidinating reactive separation process, be also applied for preparing diacetylmonoxime, expoxy propane, epoxychloropropane, dioxygen
Other gas-liquid-solid three phase catalytic reaction separation processes such as water.
Background technology
Cyclohexanone oxime is a kind of important intermediate for producing caprolactam, and oximation reaction occurs by hydroxylamine salt and cyclohexanone
It is obtained, the cyclohexanone oxime of generation obtains caprolactam through Beckmann rearrangement again.At present, cyclohexanone oxamidinating method is due to its preparation side
Method is simple, not by-product sulphur ammonium, is method that caprolactam industry is generally used without the difficult problem of environmental protection.Oximes method prepares cyclohexanone
Oxime is reacted with separation process, and metal film filter is set in reactor, after it there is catalytic reaction in cyclohexanone, cyclohexanone oxime
Separation process can be immediately completed with catalyst, compared with external filter, reduce energy consumption, but there is reactor simultaneously with gold
Belong to the matching problem of film filter, it is considered to which the heat release of reaction mass such as pipettes at the safety problem, reactor volume can not be too big, causes
Metal film can not be matched just with reactor, and separate unit reactor production capacity is low, and metal film is arranged in reactor, be not easy to dimension
Repair, due to setting metal film in reactor, mixing uniformity is low during material reaction, the conversion ratio of cyclohexanone is low, reaction mass
Local temperature is high, and accessory substance is more, causes product quality low.Therefore cyclohexanone oxamidinating reaction separating device has reaction at present
Homogeneity is poor, and cyclohexanone conversion ratio is low, and the production capacity of cyclohexanone oxime is low, the problems such as inconvenient maintenance.In order to solve the above problems, to ring
It is obvious that hexanone Ammoximation reaction separator is improved meaning.
Utility model content
The utility model is for existing cyclohexanone oxamidinating catalytic reaction and the deficiency of separation process, there is provided a kind of production capacity
Height, good effect of heat exchange, the heterogeneous catalytic reaction and UF membrane for being easy to maintenance is combined the unit.
To achieve the above object, the utility model is adopted the following technical scheme that：
A kind of heterogeneous catalytic reaction is combined the unit with UF membrane, including retort and Clear liquid tank, wherein, reaction upper end sets
Recycle stock import, catalyst charging hole and material inlet are equipped with, retort bottom is provided with recycle stock outlet and liquefied ammonia import,
Retort lateral wall is provided with purified liquor outlet, and metal film filter, guide shell, agitator, feed distribution are provided with retort
Device and liquefied ammonia distributor, circulating pump is connected with charging mixer, heat exchanger, static mixer by pipeline on external circulation line,
Static mixer is connected with recycle stock import, and recycle stock outlet is connected with circulating pump.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, on external circulation line circulating pump and charging mixer it
Between be provided with external dead-end filter or be provided with external cross-flow filter.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, and retort inner draft tube is sandwich-type guide shell or is
Coil pipe type guide shell.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, and the inoranic membrane of external cross-flow filter is ceramic membrane, its
Filtering accuracy is 30 nm~5 μm；The inoranic membrane of external dead-end filter is metal film, and its filtering accuracy is 0.05~50 μm.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, it is characterised in that external dead-end filter bottom is provided with urges
Agent is exported, and is connected with the catalyst charging hole of retort by pipeline.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, it is characterised in that metal film filter is with film in retort
Heap form is uniformly arranged on retort inner periphery, and the membrane tube filtering accuracy of metal film filter is 0.05~50 μm.
Described heterogeneous catalytic reaction is combined the unit with UF membrane, it is characterised in that pipeline charging mixer is provided with pipeline
Charge door.
The utility model can be used for cyclohexanone oxamidinating catalytic reaction and separation process, it may also be used for prepare diacetylmonoxime, ring
Other gas-liquid-solid three phase catalytic reaction separation processes such as Ethylene Oxide, epoxychloropropane, hydrogen peroxide.
The utility model obtains following beneficial effect：
1st, the utility model raw material can be directly added into retort, it is also possible to added in charging mixing, first entered in pipeline
Row pre-reaction, enters back into reactor and further reacts, and reaction mass is mixed the conversion ratio for evenly improving cyclohexanone；
2nd, using built-in metal film filter, external inorganic membrane filter can make the design of retort more reasonable, increase
Production capacity；
The 3rd, guide shell is set in the utility model in retort, the more uniform of reaction mass mixing can be made, while water conservancy diversion
Cylinder is provided with interlayer, is capable of achieving to pipette the effect of reaction heat, makes material reaction temperature equalization in retort, reduces the product of accessory substance
It is raw, can improve product quality, simultaneous reactions safety and stability reliability；
4th, the metal film filter in retort can integrally be taken out using the formal distribution of membrane stack in retort inner periphery,
It is easy to maintenance, inorganic membrane filter maintenance is put in addition also very convenient.
Brief description of the 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.
Label in accompanying drawing is represented and is meant that：
1st, retort 2, guide shell 3, metal film filter 4, recycle stock outlet 5, circulating pump 6, valve A 7,
Valve B 8, valve C 9, catalyst outlet 10, external dead-end filter 11, external cross-flow filter 12, Clear liquid tank 13,
Circulating line 14, pipeline charging mixer 15, pipeline charge door 16, heat exchanger 17, static mixer 18, catalyst add
Material mouth 19, recycle stock import 20, material inlet 21, feed distributor 22, liquefied ammonia import 23, liquefied ammonia distributor 24,
Agitator 25, built-in metal film purified liquor outlet.
Specific embodiment
Below in conjunction with the accompanying drawings and the specific embodiment that is given of accompanying drawing is further described to the utility model.
Embodiment 1
As shown in Figure 1, Figure 2, Figure 3 shows, a kind of heterogeneous catalytic reaction is combined the unit with UF membrane, is provided with retort 1 and led
Flow cartridge 2, metal film filter 3, agitator 24, feed distributor 21, liquefied ammonia distributor 23, guide shell 2 can be that sandwich-type is led
Flow cartridge or coil pipe type guide shell, metal film filter 3 are uniformly arranged on retort inner periphery, metal membrane filter in membrane stack form
The membrane tube filtering accuracy of device is 0.05~50 μm.Reaction upper end is provided with recycle stock import 19, the and of catalyst charging hole 18
Material inlet 20, retort bottom is provided with recycle stock and exports 4 and liquefied ammonia import 22, and retort lateral wall is provided with built-in metal
The purified liquor outlet 25 of film；Circulating pump 5, charging mixer 14, heat exchanger 16, static state are sequentially provided with retort outer loop pipeline
Blender 17, recycle stock outlet 4 is connected with circulating pump 5, and static mixer 17 is connected with recycle stock import 19.Outer circulating tube
A circulating line 13 is provided with road between circulating pump 5 and charging mixer 14.As shown in Figure 2 and Figure 3：Outside guide shell 2
Portion, top is more lower slightly than guide shell 2, and bottom is more slightly higher than guide shell 2, and feed distributor 21 and liquefied ammonia distributor 23 are equal to be provided with
The endless tube of even distribution hole.
The technical process that the device is used for the separation of cyclohexanone oxamidinating catalytic reaction is described below：It is cyclohexanone, hydrogen peroxide, molten
The agent tert-butyl alcohol is added from material inlet 20, and retort is entered through feed distributor 21, and catalyst is added from catalyst charging hole 18
Retort, liquefied ammonia adds retort, in the presence of agitator 24 and catalyst, ring from liquefied ammonia import 22 through liquefied ammonia distributor 23
The mixed solution of hexanone generation Ammoximation reaction generation cyclohexanone oxime, a part of cyclohexanone oxime and catalyst is along on guide shell 2
Row is descending to surrounding to top, is separated by built-in metal film filter 3, and catalyst is trapped within inside retort, another portion
The mixed solution of cyclohexanone oxime and catalyst is divided to export 4 through circulating line 13, heat exchanger 16, static mixer through recycle stock
17th, recycle stock import 19 lower the temperature fully mix after enter retort continue react, in the process of running, it is necessary to close valve 7
（B）With valve 8（C）, open valve 6（A）, the clear liquid isolated through built-in metal film filter 3 goes out through built-in metal film clear liquid
Mouth 25 enters in Clear liquid tank 12, and so circulation completes being carried out continuously for cyclohexanone oxamidinating Reaction Separation.
Embodiment 2
The circulating line between circulating pump on external circulation line 5 and charging mixer 14 replaced with the present embodiment external
Dead-end filter 10, wherein the inoranic membrane of external dead-end filter 10 is metal film, its filtering accuracy is 1 μm.External dead end mistake
Filter bottom is provided with catalyst outlet 9, is connected with the catalyst inlet 18 of retort by pipeline, and the clear liquid of dead-end filter goes out
Mouth connects Clear liquid tank 12.In the process of running, it is necessary to close valve 6（A）With valve 8（C）, open valve 7（B）, other and implementation
Example 1 is identical.
Embodiment 3
The circulating line on external circulation line between circulating pump 5 and charging mixer 14 is replaced with outward in the present embodiment
Put cross-flow filter；The inoranic membrane of wherein external cross-flow filter 11 is ceramic membrane, and its filtering accuracy is 0.5 μm, cross-flow filtration
The purified liquor outlet of device connects Clear liquid tank 12, and the filtering accuracy of built-in metal film is 0.5 μm.In the process of running, it is necessary to close valve 6
（A）With valve 7（B）, open valve 8（C）, other are same as Example 1.
Embodiment 4
The sandwich-type guide shell in retort is replaced with into coil pipe type guide shell in the present embodiment 4, other and the phase of embodiment 1
Together.
Embodiment 5
Sandwich-type guide shell in the present embodiment 5 in retort replaces with coil pipe type guide shell, other and the phase of embodiment 2
Together.
Embodiment 6
Sandwich-type guide shell in the present embodiment 6 in retort replaces with coil pipe type guide shell, other and the phase of embodiment 3
Together.
Claims (7)
1. a kind of heterogeneous catalytic reaction is combined the unit with UF membrane, including retort（1）And Clear liquid tank（12）, it is characterised in that it is anti-
Upper end is answered to be provided with recycle stock import（19）, catalyst charging hole（18）And material inlet（20）, retort bottom is provided with
Recycle stock is exported（4）With liquefied ammonia import（22）, retort side-wall outer side is provided with built-in metal film purified liquor outlet（25）, reaction
Tank（1）Inside it is provided with metal film filter（3）, guide shell（2）, agitator（24）, feed distributor（21）With liquefied ammonia distributor
（23）, circulating pump on external circulation line（5）Charging mixer is connected with by pipeline（14）, heat exchanger（16）, static mixer
（17）, static mixer（17）With recycle stock import（19）It is connected, recycle stock outlet（4）With circulating pump（5）It is connected.
2. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that on external circulation line
Circulating pump（5）And charging mixer（14）Between be provided with external dead-end filter（10）Or it is provided with external cross-flow filter
（11）.
3. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that retort Inner guide
Cylinder（2）For sandwich-type guide shell or be coil pipe type guide shell.
4. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that external cross-flow filtration
Device（11）Inoranic membrane be ceramic membrane, its filtering accuracy be 30 nm~5 μm；External dead-end filter（10）Inoranic membrane for gold
Category film, its filtering accuracy is 0.05~50 μm.
5. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that external dead-end filtration
Device bottom is provided with catalyst outlet（9）, by pipeline and the catalyst charging hole of retort（18）It is connected.
6. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that metal in retort
Film filter is uniformly arranged on retort inner periphery in membrane stack form, and the membrane tube filtering accuracy of metal film filter is 0.05~50
μm。
7. heterogeneous catalytic reaction according to claim 1 is combined the unit with UF membrane, it is characterised in that pipeline charging mixing
Device is provided with pipeline charge door（15）.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201621285147.0U CN206253115U (en) | 2016-11-28 | 2016-11-28 | A kind of heterogeneous catalytic reaction is combined the unit with UF membrane |
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| CN201621285147.0U CN206253115U (en) | 2016-11-28 | 2016-11-28 | A kind of heterogeneous catalytic reaction is combined the unit with UF membrane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096184A (en) * | 2018-09-03 | 2018-12-28 | 河北美邦工程科技股份有限公司 | A kind of preparation method of pyridine carboxylic acid class compound |
| CN110743367A (en) * | 2019-10-28 | 2020-02-04 | 南京工业大学 | Automatic filtering system and process |
| CN113828255A (en) * | 2021-10-22 | 2021-12-24 | 上海华谊（集团）公司 | Gas-liquid-solid three-phase catalytic oxidation reaction kettle and application thereof |
-
2016
- 2016-11-28 CN CN201621285147.0U patent/CN206253115U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096184A (en) * | 2018-09-03 | 2018-12-28 | 河北美邦工程科技股份有限公司 | A kind of preparation method of pyridine carboxylic acid class compound |
| CN109096184B (en) * | 2018-09-03 | 2020-07-10 | 河北美邦工程科技股份有限公司 | Preparation method of picolinic acid compound |
| 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 |
| CN113828255A (en) * | 2021-10-22 | 2021-12-24 | 上海华谊（集团）公司 | Gas-liquid-solid three-phase catalytic oxidation reaction kettle and application thereof |
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