CN206355627U - It is a kind of to be used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2 - Google Patents

It is a kind of to be used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2 Download PDF

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Publication number
CN206355627U
CN206355627U CN201621477365.4U CN201621477365U CN206355627U CN 206355627 U CN206355627 U CN 206355627U CN 201621477365 U CN201621477365 U CN 201621477365U CN 206355627 U CN206355627 U CN 206355627U
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pipeline
cyanoethyl
condensing unit
vavuum pump
spray column
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CN201621477365.4U
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郭敬强
张建民
赵耀
崔军霞
刘素强
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HEBEI YETIAN AGROCHEMICALS Co Ltd
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HEBEI YETIAN AGROCHEMICALS Co Ltd
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Abstract

It is used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2 the utility model discloses a kind of, including the vavuum pump being connected with cracking still vacuum pipe, surge tank is set between the vavuum pump and cracking still, the gas vent connection condenser of the vavuum pump, the leakage fluid dram of condenser connects recycling can by pipeline, and its exhaust outlet is connected with the bottom inlet of spray column;Packing layer is provided with inside the spray column, tower top is provided with toluene spray nozzle;The liquid outlet connection of the spray column bottom of towe absorbs groove, and the gas outlet of the spray column overhead passes through the air inlet of pipeline communication to adsorption tower, the gas outlet connection chimney of adsorption tower.The utility model has carried out sufficient condensation and recovery to the material gas produced by cracking, greatly improves the recycling efficiency of material, reduces production cost;Material gas is by multiple condensation, absorption and purifies, and the gas of outer row does not have organic substance, without smell, and air is not polluted, very environmentally friendly.

Description

A kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes
Technical field
The utility model is related to a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes, belongs to Technical field of chemical synthesis.
Background technology
2-vhloro-5-chloromethylpyridine(2-chloro-chloromethylpyridine, abbreviation CCMP) it is new and effective The key intermediate of pesticide imidacloprid (Imidacloprid) and acetamiprid (NI -25), be also in this class pesticide molecule most The part of insecticidal activity, and pass through its alkylated reaction, with after heterocycle N-H condensation reaction and ammonification with 1- nitros- The reaction of 2,2- double (sulfidomethyl) ethene, can also prepare a series of new insecticidal/acaricidal agents, be the important of synthetic pesticide and medicine Intermediate.
Current domestic production 2-vhloro-5-chloromethylpyridine mainly uses cyclopentadiene technique, with cyclopentadiene and third Olefine aldehydr is raw material, and 2-vhloro-5-chloromethylpyridine is finally given by series reaction.Its reaction scheme is:
Wherein, three-step reaction process is:2- cyanoethyl -5- Norbornene-2-carboxaldehydes are split at 210 DEG C ~ 235 DEG C Solution, generation 2- methylene -4- cyanobutyraldehydes and cyclopentadiene;Cracking process need keep negative pressure state, make product 2- methylene- 4- cyanobutyraldehydes and cyclopentadiene are steamed in time, promote cracking reaction constantly to carry out to the right.
In conventional cracking reaction system, vavuum pump is connected with cracking still, and surge tank is directly connected to after vavuum pump, buffering Tank connects the condenser using chilled brine as temperature-reducing medium, and the product in gas is condensed out and reclaimed.But this is filled Put still have some defects, mainly including it is following some:1. material gas temperature is very high, and part is had under vacuum directly Into in surge tank, cyclopentadiene is possible to polymerize at high temperature, can produce more gather in surge tank over time Compound;2. after the buffered tank of material gas, its temperature is still higher, and directly the brine condenser with -15 DEG C is contacted, and causes condensation The thermal shock of device, reduces the life-span of condenser;3. the moisture in material gas, can be reduced cold in condenser tubulation shallow freezing Solidifying effect;4. directly and atmosphere, partial material gas passes through that surge tank is directly outer to be arranged to surge tank, wastes reaction product, increases Plus while production cost, environment is polluted.
The content of the invention
To solve the above mentioned problem that prior art is present, the purpose of this utility model is to provide a kind of for 2- cyanogen second The vacuum condensing unit of base -5- Norbornene-2-carboxaldehydes cracking, the device has been carried out sufficiently to the material gas produced by cracking Condensation and recovery, improve the recycling efficiency of material, reduce production cost.
In order to solve the above technical problems, the technical scheme that the utility model is used is:
One kind is used for the-vacuum condensing unit of cyanoethyl -- ENB -- aldehyde lyase, including with cracking still vacuum pipe The vavuum pump being connected, sets surge tank, the gas vent connection condensation of the vavuum pump between the vavuum pump and cracking still Device, the leakage fluid dram of condenser connects recycling can by pipeline, and its exhaust outlet is connected with the bottom inlet of spray column;The spray Packing layer is provided with inside tower, tower top is provided with toluene spray nozzle;The liquid outlet connection of the spray column bottom of towe absorbs groove, absorbs groove The spray liquid entrance for spraying column overhead is also connected by circulating pump;The gas outlet of the spray column overhead passes through pipeline communication to suction The air inlet of attached tower, the gas outlet connection chimney of adsorption tower, is additionally provided with adsorption tower gas outlet for providing drainage power Air-introduced machine;
The medium inlet connection water temperature of the condenser is 4 ~ 6 DEG C of CWS road, media outlet connection cooling Water water return pipeline.
Further improvement of the utility model is:The discharging opening of the buffering bottom of the tube connects recycling can by pipeline; The outlet being connected with recycling can is also equipped with the housing of the vavuum pump.
Further improvement of the utility model is:The absorption groove also connects saturation liquid storage tank, saturated solution by pipeline Storage tank is communicated to toluene recovery workshop section.Further improvement of the utility model is:Liquid level is provided with the saturation liquid storage tank Meter.
Further improvement of the utility model is:The adsorption tower is activated carbon adsorber.
Further improvement of the utility model is:The recycling can purifies workshop section by pipeline and cyclopentadiene and is connected It is logical, in the exit of recycling can, feeding engine is set.
By adopting the above-described technical solution, the technological progress that the utility model is obtained is:
The utility model provides a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes, right Material gas produced by cracking has carried out sufficient condensation and recovery, greatly improves the recycling efficiency of material, drops Low production cost;Material gas is by multiple condensation, absorption and purifies, and the gas of outer row does not have organic substance, without smell, Air is not polluted, it is very environmentally friendly.
Surge tank is arranged between vavuum pump and cracking still by the utility model, and material gas is carried out tentatively in surge tank Condense and preliminary cooling, condense in vavuum pump and then further and cool;Then, on-condensible gas enter back into condenser carry out it is cold But, the thermal shock to condenser is greatly reduced, the condenser life-span is extended;Meanwhile, the cooling water temperature that condenser is used is 4 DEG C ~ 6 DEG C, cyclopentadiene can be fully condensed, the aqueous vapor in fixed gas will not be made to be frozen on tubulation surface again, can obtain long-term steady Fixed condensation effect.
The on-condensible gas discharged by condenser enters spray column and carries out toluene spray-absorption, and remaining cyclopentadiene is in spray It is completely absorbed in tower;Toluene spray liquid cyclic absorption, it is progressively enriched with, toluene recovery workshop section is sent into after saturation to be achieved and is returned Receive, cyclopentadiene is reused as reaction raw materials, and toluene is recycled as spray liquid, greatly reduces the wave of material Take.
Brief description of the drawings
Fig. 1 is connection diagram of the present utility model;Arrow in figure indicates the flow direction of gas;
Wherein, 1, cracking still, 2, surge tank, 3, vavuum pump, 4, condenser, 41, recycling can, 42, feeding engine, 5, spray Tower, 51, absorb groove, 52, saturation elution liquid storage tank, 53, circulating pump, 6, adsorption tower, 61, air-introduced machine, 7, chimney, 81, cooling water Water pipeline, 82, CWR road.
Embodiment
Describe the utility model in detail below with reference to the accompanying drawings.
A kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes, as shown in figure 1, including with splitting The vavuum pump 3 that the solution vacuum pipe of kettle 1 is connected, sets surge tank 2, the bottom of separator tube 2 between the vavuum pump 3 and cracking still 1 Discharging opening pass through pipeline connect recycling can 41.The gas vent connection condenser 4 of the vavuum pump 3;In the condenser 4 Cooling medium is 4 ~ 6 DEG C of the cooling water from CWS road, the medium inlet connection CWS of condenser 4 Road 81, media outlet connection CWR road 82;The leakage fluid dram of condenser 4 connects recycling can 41 by pipeline, and it is vented Mouth is connected with the bottom inlet of spray column 5.The spray column 5 is toluene spray column, and packing layer is provided with tower, and tower top is set There is toluene spray nozzle.The liquid outlet connection of the bottom of towe of spray column 5 absorbs groove 51, absorbs groove 51 and also connects spray by circulating pump The spray liquid entrance of the tower top of tower 5;The gas outlet of the tower top of spray column 5 passes through the air inlet of pipeline communication to adsorption tower 6, absorption The gas outlet connection chimney 7 of tower 6, is additionally provided with the air-introduced machine 61 for providing drainage power at the gas outlet of adsorption tower 6.
The outlet being connected with recycling can 41 is additionally provided with the housing of the vavuum pump 3, is condensed out in vavuum pump 3 Hydrops be discharged into time in recycling can 41, prevent the corrosion to the pump housing and the influence to vacuum.
The accumulator tank 41 is used for the cyclopentadiene for receiving to condense out, and its source includes:1. the condensate liquid in surge tank, 2. the condensate liquid in vacuum pump case, the condensate liquid 3. produced in condenser;Condensed by this three step, most cyclopentadiene Be condensed collection, and the cyclopentadiene that residue is not condensed is dissolved in spray column by toluene.Cyclopentadiene in accumulator tank 41 is cold Lime set sent under the driving of feeding engine 42 cyclopentadiene purification workshop section, by purification, can as 5- Norbornene-2-carboxaldehydes system Standby raw material is used.
Sample tap is set on the absorption groove 51, staff detects the concentration of toluene spray liquid by sample tap in time, It is discharged into immediately in saturation liquid storage tank 52 after saturation, and adds pure toluene or apply mechanically toluene continuation spray, absorb.
The outlet of the circulating pump 53 connects two branch lines, the spray at the top of the first branch line connection spray column 5 Liquid entrance, for sending the toluene absorbed in groove back to tower top, repeatedly spray-absorption;Second branched pipe road is communicated to saturation liquid storage tank 52, the toluene solution for keeping in saturation sets liquid level gauge on saturation liquid storage tank 52, and the toluene solution of saturation is admitted to toluene and returned Section of knocking off carries out recovery separation, and the cyclopentadiene isolated is reused as the preparing raw material of 5- Norbornene-2-carboxaldehydes, separates The toluene gone out continues to apply mechanically as spray liquid.
The course of work and principle of the present utility model are:
Material gas is discharged by cracking still under vacuum, and row buffering, a part of cyclopentadiene quilt are entered in surge tank Condense out, drained into via the discharging opening at surge tank bottom in tourie 41;On-condensible gas is sent into condenser through vavuum pump and carried out Condensation.Cooling medium in condenser is the cooling water that temperature is 4 ~ 6 DEG C, within the condenser under most cyclopentadiene condensations Come, be discharged into through pipeline in tourie 41, condensation fixed gas is admitted to spray column bottom inlet through pipeline, and toluene is pushed up by spray column 5 Portion is sprayed downwards, and condensation fixed gas is flowed up by bottom of towe, fully contact, realize that material is fully absorbed in condensation fixed gas, Ejecting liquid is drained into absorption groove and the circulated sprinkling in the presence of circulating pump by the liquid outlet of bottom of towe;Tail gas is sprayed by spraying Column overhead is directly discharged into adsorption tower, is provided with multilayer charcoal absorption plate in adsorption tower, tail gas through charcoal absorption plate, its After the micro organic gas of entrainment is fully absorbed, arranged directly in the presence of air-introduced machine outside chimney.
The foregoing is only preferred embodiment of the present utility model, it is all according to present utility model application the scope of the claims done it is equal Deng change and modification, it should all belong to covering scope of the present utility model.

Claims (6)

1. it is a kind of for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes crack vacuum condensing unit, including with cracking still(1)Vacuum The vavuum pump that pipeline is connected(3), it is characterised in that:The vavuum pump(3)With cracking still(1)Between surge tank is set(2), institute State vavuum pump(3)Gas vent connection condenser(4), condenser(4)Leakage fluid dram recycling can is connected by pipeline(41), its Exhaust outlet and spray column(5)Bottom inlet be connected;The spray column(5)Inside is provided with packing layer, and tower top is provided with toluene Spray nozzle;The spray column(5)The liquid outlet connection of bottom of towe absorbs groove(51), absorb groove(51)Also connected and sprayed by circulating pump Tower(5)The spray liquid entrance of tower top;The spray column(5)The gas outlet of tower top passes through pipeline communication to adsorption tower(6)Air inlet Mouthful, adsorption tower(6)Gas outlet connection chimney(7), in adsorption tower(6)It is additionally provided with gas outlet for providing drainage power Air-introduced machine(61);
The condenser(4)Medium inlet connection water temperature be 4 ~ 6 DEG C of CWS road(81), media outlet connects cold But water water return pipeline(82).
2. a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes according to claim 1, It is characterized in that:The surge tank(2)The discharging opening of bottom connects recycling can by pipeline(41);The vavuum pump(3)Shell It is also equipped with and recycling can in vivo(41)The outlet being connected.
3. a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes according to claim 1, It is characterized in that:The absorption groove(51)Saturation liquid storage tank is also connected by pipeline(52), saturation liquid storage tank(52)It is communicated to first Benzene recycle section.
4. a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes according to claim 3, It is characterized in that:The saturation liquid storage tank(52)On be provided with liquid level gauge.
5. a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes according to claim 1, It is characterized in that:The adsorption tower(6)For activated carbon adsorber.
6. a kind of vacuum condensing unit cracked for 2- cyanoethyl -5- Norbornene-2-carboxaldehydes according to claim 1, It is characterized in that:The recycling can(41)Workshop section is purified by pipeline and cyclopentadiene to be connected, in recycling can(41)Outlet Place sets feeding engine(42).
CN201621477365.4U 2016-12-30 2016-12-30 It is a kind of to be used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2 Active CN206355627U (en)

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CN201621477365.4U CN206355627U (en) 2016-12-30 2016-12-30 It is a kind of to be used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2

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CN201621477365.4U CN206355627U (en) 2016-12-30 2016-12-30 It is a kind of to be used for the vacuum condensing unit of the aldehyde lyase of 2 cyanoethyl, 5 ENB 2

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003057A (en) * 2017-11-30 2018-05-08 庆阳凯威尔能源化工有限公司 A kind of continuous cracking production method of 2- methylene -4- cyanobutyraldehydes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003057A (en) * 2017-11-30 2018-05-08 庆阳凯威尔能源化工有限公司 A kind of continuous cracking production method of 2- methylene -4- cyanobutyraldehydes

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