CN203764270U - Device capable of preventing solvent volatilization and fast recovering palladium and carbon - Google Patents
Device capable of preventing solvent volatilization and fast recovering palladium and carbon Download PDFInfo
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- CN203764270U CN203764270U CN201420110509.7U CN201420110509U CN203764270U CN 203764270 U CN203764270 U CN 203764270U CN 201420110509 U CN201420110509 U CN 201420110509U CN 203764270 U CN203764270 U CN 203764270U
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- filter
- valve
- hydrogenation reaction
- reaction kettle
- palladium carbon
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Abstract
The utility model provides a device capable of preventing solvent volatilization and fast recovering palladium and carbon. The device comprises a hydrogenation reaction kettle, a filter and a liquid storage tank, wherein a pressure filter pump is arranged between the hydrogenation reaction kettle and the filter, and the liquid storage tank and the filter are connected with each other; the filter comprises an upper cover and a tank body, a screen drum is arranged on the inner side of the tank body, and a filter bag is arranged on the inner side of the screen drum. Through the pressure filter pump and the filter, palladium and carbon can be fast recovered by pumping and filtering, and as the whole process is in a closed state, the volatilization of a solvent can be effectively prevented.
Description
Technical field
The utility model relates to chemical industry and manufactures field, relates in particular to a kind of device of the quick recovery palladium carbon that prevents solvent evaporates.
Background technology
At new and effective low toxic pesticide indoxacarb intermediate 2-benzyloxy carboxyl-7-chlorine indeno [1,2-P] [1,3,4] oxadiazines-2,4a(3H, 5H) in the production technology of-4a-carboxylate methyl ester, use that palladium carbon makees catalyst and ethyl acetate makees solvent.After completing, hydrogenation reaction needs the palladium-carbon catalyst in solution to reclaim.As shown in Figure 3, the solidliquid mixture in hydrogenation reaction kettle 21 enters suction filtration case 23 through valve 22 to the retracting device of using in prior art, and wherein in solidliquid mixture, palladium carbon is solid, and other materials are all dissolved in ethyl acetate solvent; Filter bag 24 is set in suction filtration case 23, and the palladium carbon in described solidliquid mixture is stayed in filter bag 24 after filtration; The filter 25 that solution arranges near suction filtration case 23 bottoms through filter bag 24 belows through filter bag 24 flows into suction filtration case 23 bottoms, and suction filtration case 23 is connected with vacuum filtration tank 27 by valve 26, and the solution filtering out deposits in vacuum filtration tank 27.After solidliquid mixture in hydrogenation reaction kettle 21 has filtered, the solid palladium carbon obtaining in suction filtration case 23 is poured out to recovery.Because ethyl acetate has very high volatility, in the process of making suction filtration case 23 He in suction filtration tank 27 vacuum filtration processes, can vapor away a large amount of ethyl acetate, cause the wasting of resources; And whole suction filtration process is consuming time more of a specified duration, taking the hydrogenation reaction kettle of 3000L capacity and the suction filtration pipeline of 50mm diameter as example, once complete suction filtration needs consuming time more than one hour.
Utility model content
After the technical problems to be solved in the utility model is to provide a kind of hydrogenation reaction and completes, can reclaim fast palladium carbon and prevent the device of solvent evaporates.
For solving the problems of the technologies described above, the utility model provides a kind of device of the quick recovery palladium carbon that prevents solvent evaporates, comprise hydrogenation reaction kettle, filter and fluid reservoir, between described hydrogenation reaction kettle and filter, filter pressing pump is set, described fluid reservoir is connected with filter; Described filter comprises upper cover and casing, and described box inside arranges screen drum, and described screen drum inner side arranges filter bag; The first valve is set between described hydrogenation reaction kettle and filter pressing pump, the second valve is set between described filter and fluid reservoir, described the first valve and the second valve are up-down structure.
Further, transparent visor is set between described hydrogenation reaction kettle and filter pressing pump, described visor is arranged between the first valve and the second valve.The mixture of can handled easily person grasping in time in hydrogenation reaction kettle be set whether fall into smoothly hydraulic pump of transparent visor herein.Fall when no longer including material in visor, operator can judge that the solidliquid mixture in hydrogenation reaction kettle all falls into hydraulic pump, conveniently carries out next step operation arrangement.
Further, described filter is stainless steel tubular structure.On filter box-body, be stamped upper cover and seal, and whole palladium carbon removal process do not need to open upper cover, thereby reduced the volatilization of solvent.
Further, the U-shaped structure that described screen drum is bottom lock, surrounding and bottom arrange sieve aperture, and described sieve diameter is 10mm.Screen drum is played a supporting role to filter bag, and the sieve aperture inflow filter lower box that simultaneously solution can be on screen drum, enters fluid reservoir through pipeline.
Further, described filter bag is 1000 order filter bags.The filtering holes of filter bag is excessive, cannot play the effect of filtering palladium charcoal, and filtering holes is too small, can affect passing through of liquid, and the utility model is 1000 order filter bags preferably.
Further, the capacity of described hydrogenation reaction kettle and described fluid reservoir is consistent.Because fluid reservoir is for depositing the solution after filtration, so the two capacity unanimously can ensure enough to deposit, be unlikely to again to cause because fluid reservoir is excessive waste.
The beneficial effects of the utility model are: by filter pressing pump and filter are set, the pump of employing is played filtration can reclaim palladium carbon fast, and whole process is closed state, can effectively prevent the volatilization of solvent.Taking the hydrogenation reaction kettle of 3000L capacity as example, the flow of described press pump machine is 20 ~ 30
/ h, complete the 5min that is applied for of a filtered and recycled, greatly shorten the time, thereby avoid vacuum to take away and suction filtration case solvent flashing, simultaneously easy and simple to handle, every batch of complete palladium-carbon catalyst that can reclaim 2 ~ 3kg of press filtration, as long as open filter lid, pour out the palladium-carbon catalyst in filter bag, because filter sock is little, press filtration catalyst attrition is out little.
Brief description of the drawings
Fig. 1 is the overall structure schematic diagram of the utility model embodiment;
Fig. 2 is the structural representation of Fig. 1 middle filtrator (in dotted line frame);
Fig. 3 is palladium carbon retracting device structural representation of the prior art.
Description of reference numerals:
1-hydrogenation reaction kettle, the 2-the first valve, 3-visor, the 4-the second valve, 5-filter pressing pump, 6-filter, 61-upper cover, 62-casing, 63-filter bag, 64-screen drum, the 7-the three valve, 8-fluid reservoir, 21-hydrogenation reaction kettle, 22-valve, 23-suction filtration case, 24-filter bag, 25-filter, 26-valve, 27-suction filtration tank.
Detailed description of the invention
In order to make the purpose of this utility model, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the utility model is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain the utility model, and be not used in restriction the utility model.
The device of the quick recovery palladium carbon that prevents solvent evaporates as shown in Figure 1, comprise hydrogenation reaction kettle 1, hydrogenation reaction kettle 1 is connected with visor 3 by the first valve 2, visor 3 is connected with filter pressing pump 5 by the second valve 4, filter pressing pump 5 is connected with filter 6, and filter 6 is connected with fluid reservoir through the 3rd valve 7.
As shown in Figure 2, filter 6 comprises upper cover 61, casing 62, filter bag 63 and screen drum 64.Filter 6 is stainless steel tubular structure.On filter box-body 62, be stamped upper cover 61 and seal, and whole palladium carbon removal process do not need to open upper cover 61, every batch of complete filter cover 61 of opening of press filtration, pours out the palladium-carbon catalyst of 63 li of filter bags, thereby has reduced the volatilization of solvent.Wherein filter bag 63 is 1000 order filter bags.The filtering holes of filter bag 63 is excessive, cannot play the effect of filtering palladium charcoal, and filtering holes is too small, can affect passing through of liquid, and the present embodiment is 1000 order filter bags preferably.The U-shaped structure that screen drum 64 is bottom lock, surrounding and bottom arrange sieve aperture, and described sieve diameter is 10mm.
At new and effective low toxic pesticide indoxacarb intermediate 2-benzyloxy carboxyl-7-chlorine indeno [1,2-P] [1,3,4] oxadiazines-2,4a(3H, 5H) in the production technology of-4a-carboxylate methyl ester, use that palladium carbon makees catalyst and ethyl acetate makees solvent.In hydrogenation reaction kettle 1, carry out the complete solidliquid mixture of hydrogenation reaction, now, except palladium-carbon catalyst is solid, other materials are all dissolved in solvent.Whether described solidliquid mixture falls into filter pressing pump 5 through the first valve 2 and the second valve 4, in this process, can observe at any time mixture by visor 3 and fall.Mixture is pressed in filter 6 through filter pressing pump 5, palladium-carbon catalyst is stayed in filter bag 63 through filter bag 63, casing 62 bottoms of the sieve aperture inflow filter 6 of solution on screen drum 64, then enter fluid reservoir 8 through the 3rd valve 7 and pipeline, carry out the recovery of solvent by fluid reservoir 8.
In the present embodiment, taking the fluid reservoir of the hydrogenation reaction kettle of 3000L capacity, 3000L capacity as example, the flow of filter pressing pump 5 is 20 ~ 30
/ h, complete the 5min that is applied for of a filtered and recycled, greatly shorten the time, thereby avoid vacuum to take away and suction filtration case solvent flashing, simultaneously easy and simple to handle, every batch of complete palladium-carbon catalyst that can reclaim 2 ~ 3kg of press filtration, as long as open filter lid, pour out the palladium-carbon catalyst in filter bag, because the worry hole of filter sock is little, press filtration catalyst attrition is out little.
The disclosed technological means of the utility model scheme is not limited only to the disclosed technological means of above-mentioned embodiment, also comprises the technical scheme being made up of above technical characterictic.
Claims (6)
1. the device that prevents the quick recovery palladium carbon of solvent evaporates, comprises hydrogenation reaction kettle, filter and fluid reservoir, it is characterized in that: between described hydrogenation reaction kettle and filter, filter pressing pump is set, described fluid reservoir is connected with filter; Described filter comprises upper cover and casing, and described box inside arranges screen drum, and described screen drum inner side arranges filter bag; The first valve is set between described hydrogenation reaction kettle and filter pressing pump, the second valve is set between described filter and fluid reservoir, described the first valve and the second valve are up-down structure.
2. the device of the quick recovery palladium carbon that prevents solvent evaporates as claimed in claim 1, is characterized in that: transparent visor is set between described hydrogenation reaction kettle and filter pressing pump, and described visor is arranged between the first valve and the second valve.
3. the device of the quick recovery palladium carbon that prevents solvent evaporates as claimed in claim 1, is characterized in that: described filter is stainless steel tubular structure.
4. the device of the quick recovery palladium carbon that prevents solvent evaporates as claimed in claim 1, is characterized in that: the U-shaped structure that described screen drum is bottom lock, and surrounding and bottom arrange sieve aperture, and described sieve diameter is 10mm.
5. the device of the quick recovery palladium carbon that prevents solvent evaporates as claimed in claim 1, is characterized in that: described filter bag is 1000 order filter bags.
6. the device of the quick recovery palladium carbon that prevents solvent evaporates as claimed in claim 1, is characterized in that: the capacity of described hydrogenation reaction kettle and described fluid reservoir is consistent.
Priority Applications (1)
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CN201420110509.7U CN203764270U (en) | 2014-03-12 | 2014-03-12 | Device capable of preventing solvent volatilization and fast recovering palladium and carbon |
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CN201420110509.7U CN203764270U (en) | 2014-03-12 | 2014-03-12 | Device capable of preventing solvent volatilization and fast recovering palladium and carbon |
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CN201420110509.7U Expired - Fee Related CN203764270U (en) | 2014-03-12 | 2014-03-12 | Device capable of preventing solvent volatilization and fast recovering palladium and carbon |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112057929A (en) * | 2020-09-07 | 2020-12-11 | 江苏九九久科技有限公司 | Method for automatically separating and recycling solid catalyst in liquid reaction |
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2014
- 2014-03-12 CN CN201420110509.7U patent/CN203764270U/en not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112057929A (en) * | 2020-09-07 | 2020-12-11 | 江苏九九久科技有限公司 | Method for automatically separating and recycling solid catalyst in liquid reaction |
CN112057929B (en) * | 2020-09-07 | 2022-05-31 | 江苏九九久科技有限公司 | Method for automatically separating and recycling solid catalyst in liquid reaction |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140813 Termination date: 20150312 |
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EXPY | Termination of patent right or utility model |