CN107043349A - A kind of 5-chloromethyl pyridine refining method of 2 chlorine 5 - Google Patents
A kind of 5-chloromethyl pyridine refining method of 2 chlorine 5 Download PDFInfo
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- CN107043349A CN107043349A CN201611209934.1A CN201611209934A CN107043349A CN 107043349 A CN107043349 A CN 107043349A CN 201611209934 A CN201611209934 A CN 201611209934A CN 107043349 A CN107043349 A CN 107043349A
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/61—Halogen atoms or nitro radicals
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Abstract
The invention discloses a kind of 5-chloromethyl pyridine refining method of 2 chlorine 5, it is characterized in that：This method comprises the following steps：（1）Dicyclopentadiene（DCP）Cracking；（2）5 ENBs（CN）Synthesis；（3）The alkene of 2 aldehyde of cycloheptyl, 2 β propionitrile 5（CCN）Addition, de- benzene, cracking；（4）The allyl acetonitrile of 4 aldehyde radical 4（CFN）Chlorination；（5）The dichloro valeronitrile of 4 aldehyde radical 4,5（CCC）Cyclization；（6）Hydrolysis, neutralization；（7）The PMC of 2 chlorine 5（CCMP）Take off benzene, refine.
Description
Technical field
The present invention relates to 2-vhloro-5-chloromethylpyridine process for purification technical field, specially a kind of chloro- 5- chloromethyls pyrroles of 2-
Pyridine process for purification.
Background technology
2-vhloro-5-chloromethylpyridine is the important intermediate of anabasine pesticide imidacloprid, buttocks worm miaow and Nitenpyram etc.,
They have wide spectrum, efficiently, low toxicity, low-residual the features such as.In -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene (CCN) in known technology
Addition this step needs substantial amounts of saturated nacl aqueous solution to be washed, and the technology can produce substantial amounts of brine waste, yield compared with
Low, accessory substance is more, and product purity is not high.
The content of the invention
It is an object of the invention to provide a kind of 2-vhloro-5-chloromethylpyridine process for purification, to solve above-mentioned background technology
The problem of middle proposition.
To achieve the above object, the present invention provides following technical scheme：A kind of 2-vhloro-5-chloromethylpyridine process for purification,
This method comprises the following steps：
(1) dicyclopentadiene (DCP) is cracked；
(2) 5- ENBs (CN) are synthesized；
(3) -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene (CCN) addition, de- benzene, cracking；
(4) 4- aldehyde radicals-allyl acetonitrile (CFN) chlorination；
(5) 4- aldehyde radicals -4,5- dichloro valeronitrile (CCC) cyclization；
(6) hydrolyze, neutralize；
(7) 2-vhloro-5-chloromethylpyridine (CCMP) takes off benzene, refined.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (1) dicyclopentadiene (DCP) splits
Solution method is, when the oil outlet temperature of vaporizes kettle and thin film evaporator reaches 240 degree, opens DCP feed pumps, opens thin film evaporation
Device and vaporizes kettle stirring, feed to cracking system, when there is cyclopentadiene (CP) extraction, CP contents obtained by timely sampling analysis,
Content requirement is more than 97%.It is 50 DEG C ± 5 DEG C to control tower top top temperature, and it is -5 DEG C~+10 DEG C to adopt outlet temperature, and the CP of collection is supplied
Next unit is standby.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (2) 5- ENBs (CN) conjunction
It is, by 750 kilograms of methacrylaldehyde for entering in CN synthesis reactors, to open the recirculated water turnover valve of synthesis reactor cooling coil, open into method
Dynamic synthesis reactor stirring, is slowly added dropwise 870 kilograms of CP into kettle, and by dropping temperature control at 40 DEG C~45 DEG C, completion of dropwise addition continues
Insulation reaction sampling analysis after 5~6 hours, methacrylaldehyde≤0.5% is reaction end, react 5- ENBs (CN) for next
Unit is standby.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, the described β-the third of step (3) cycloheptyl -2- aldehyde -2
Nitrile -5- alkene (CCN) addition, de- benzene, cleavage method be, enters to add by 3000 kilograms of toluene (TOL) and 380 kilograms of acrylonitrile (AN) are standby
Into in kettle, start reactor stirring, be warming up to 25 DEG C, add after 20 kilograms of tert-butyl alcohols and 8 kilograms of potassium hydroxide to addition kettle
560 kilograms of CN of middle dropwise addition, controlling reaction temperature is at 25 DEG C~28 DEG C, and the follow-up continuous insulation reaction of completion of dropwise addition is sampled after 1 hour divides
Analysis, CN contents≤1.0%, which reacts, to be terminated, and reacts to obtain -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene (CCN) toluene solution；Start film to take off
The de- benzene vacuum pump set of molten system, starts the cloth motor of thin film evaporator, the feed pump of CCN- toluene liquid is opened, to film
Evaporation feed liquor, opens the heating steam of thin film evaporator, it is ensured that CCN concentrate drop temperatures are maintained at 60 DEG C~85 DEG C；Open
Oilless vertical vacuum pump, puts into CCN concentrates (1300 kilograms) in CFN cracking stills, opens conduction oil import and export valve, opens
Begin slowly to heat up, infinite reflux when pushing up temperature to 90 DEG C to the fraction that hits is started, until kettle temperature to 200 DEG C, what no extraction of tower top
When stop extraction；Vacuum breaker emptying, slag tap while hot, obtain about 390 kilograms of cut in 4- aldehyde radicals-allyl acetonitrile (CFN), content >=
82% is standby for next unit.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (4) 4- aldehyde radicals-allyl acetonitrile
(CFN) chlorination is to put into chlorination tank 900 kilograms of dimethylformamides (DMF) and 900 kilograms of CFN, start chlorination
Kettle is stirred and circulating pump, and material is cooled into 5 DEG C, opens the outlet valve of chlorine cylinder, about 650 kilograms are passed through into system
CL2, control material temperature is at 0 DEG C~5 DEG C, until reaction reaches terminal, the material that chlorination is completed warms naturally to 10 DEG C~l 5
DEG C insulation is transferred to CCC degassing kettles after 1 hour, then is incubated 1 hour, decompression degassing, end temperature≤30 DEG C, degassing supplies ring after terminating
Post is closed to use.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (5) 4- aldehyde radicals -4,5- dichloro penta
Nitrile (CCC) cyclisation method is 2000kg TOL (moisture content be less than 0.1%) to be pumped into CCC cyclization kettles and half crowd of CCC-DMF is molten
Liquid, starts the stirring of cyclization kettle, and temperature in kettle is risen into 90 DEG C starts that 350 kilograms of POCl3s (POCL3) are added dropwise, and controls the temperature to be
90 ± 2 DEG C, time for adding is 3.5~4 hours, and sampling analysis is started within 1 hour in 90 ± 2 DEG C of insulation reactions after completion of dropwise addition, when
Terminate reaction during CCC contents≤2%, be cooled to 75 DEG C~80 DEG C degree blowings and enter hydrolysis and neutralize kettle.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (6) hydrolysis, neutralization method be,
Start the stirring that hydrolysis neutralizes kettle, material in kettle be cooled to 35 DEG C~45 DEG C, 1200 kg of water are added dropwise into kettle and are hydrolyzed,
The water of lower floor is put into sour water surge tank, upper toluene layer is stayed in kettle, soda ash solution is added dropwise into kettle, and measure material in time
PH value, pH value should=8, then proceed to stirring 30 minutes, repetition measurement pH value reaches requirement, then stop stirring, stand 60 minutes points
Layer, enters neutral water storage tank, toluene is put into CCP- toluene solution surge tanks by the moisture of lower floor.
It is preferred that, described 2-vhloro-5-chloromethylpyridine process for purification, described step (7) 2-vhloro-5-chloromethylpyridine
(CCMP) it is to start the de- benzene vacuum pump set of film desolventizing system to take off benzene, process for purification, and crawl starts CCP thin film evaporators
Motor, thin film evaporator is pumped into by the toluene solutions of CCP mono-, it is ensured that CMCP drop temperatures are maintained at 60 DEG C~75 DEG C, and precipitation is good
CCP be pumped into bis- de- benzene kettles of CCMP.Precipitation is depressurized to last, it is desirable to kettle temperature no more than 95 DEG C, sampling analysis toluene level≤
5% terminates, and cools standby to 60 DEG C~70 DEG C blowing meterings, takes out thick CCMP550 kilograms and enter in 500L distillation stills.Open chuck
Steam heat up, required according to finished product content, before accurately cutting, in evaporate, when kettle temperature reaches 160 DEG C~165 DEG C, now without rear fraction
When out, jacket steam valve is closed, begin to rehearse slag air-introduced machine, be slowly opened into and all open after the sufficient atmospheric valve several seconds, immediately all
The rapid deslagging of bottom valve is opened, while hot goes out slag in kettle to the greatest extent.
Compared with prior art, the beneficial effects of the invention are as follows：Production cost is reduced, waste water, the production of solid waste is reduced
Raw amount, improves conversion ratio.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
The present invention provides a kind of technical scheme：
Embodiment 1：
A kind of 2-vhloro-5-chloromethylpyridine process for purification, this method comprises the following steps：
(1) dicyclopentadiene (DCP) is cracked；
(2) 5- ENBs (CN) are synthesized；
(3) -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene (CCN) addition, de- benzene, cracking；
(4) 4- aldehyde radicals-allyl acetonitrile (CFN) chlorination；
(5) 4- aldehyde radicals -4,5- dichloro valeronitrile (CCC) cyclization；
(6) hydrolyze, neutralize；
(7) 2-vhloro-5-chloromethylpyridine (CCMP) takes off benzene, refined.
Embodiment 2：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1, described step (1) dicyclopentadiene
(DCP) cleavage method is when the oil outlet temperature of vaporizes kettle and thin film evaporator reaches 240 degree, to open DCP feed pumps, open
Thin film evaporator and vaporizes kettle stirring, feed to cracking system, when there is cyclopentadiene (CP) extraction, obtained by timely sampling analysis
CP contents, content requirement is more than 97%.It is 50 DEG C ± 5 DEG C to control tower top top temperature, adopts outlet temperature for -5 DEG C~+10 DEG C, receives
The CP of collection is standby for next unit.
Embodiment 3：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1 or 2, described step (2) 5- ENBs
(CN) synthetic method is, by 750 kilograms of methacrylaldehyde for entering in CN synthesis reactors, to open the recirculated water turnover valve of synthesis reactor cooling coil
Door, starts synthesis reactor stirring, 870 kilograms of CP is slowly added dropwise into kettle, and by dropping temperature control at 40 DEG C~45 DEG C, knot is added dropwise
Beam, continuation insulation reaction sampling analysis after 5~6 hours, methacrylaldehyde≤0.5% is reaction end, reacts to obtain 5- ENBs
(CN) it is standby for next unit.
Embodiment 4：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1 or 2 or 3, described step (3) cycloheptyl -2-
The β of aldehyde-2-propionitrile-5- alkene (CCN) addition, de- benzene, cleavage method are, by 3000 kilograms of toluene (TOL) and 380 kilograms of acrylonitrile
(AN) for entering in addition kettle, start reactor stirring, be warming up to 25 DEG C, add 20 kilograms of tert-butyl alcohols and 8 kilograms of potassium hydroxide
560 kilograms of CN are added dropwise in backward addition kettle, controlling reaction temperature is at 25 DEG C~28 DEG C, and the follow-up continuous insulation reaction 1 of completion of dropwise addition is small
When after sampling analysis, the reaction of CN contents≤1.0% terminates, and reacts to obtain -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene (CCN) toluene solution；
Start the de- benzene vacuum pump set of film desolventizing system, start the cloth motor of thin film evaporator, open the charging of CCN- toluene liquid
Pump, feeds to thin film evaporator, opens the heating steam of thin film evaporator, it is ensured that CCN concentrate drop temperatures are maintained at 60 DEG C
~85 DEG C；Open oilless vertical vacuum pump, in CFN cracking stills put into CCN concentrates (1300 kilograms), open conduction oil into and out of
Mouth valve, starts slow heating, starts the fraction that hits when infinite reflux is to top temperature to 90 DEG C, until kettle temperature is to 200 DEG C, tower top does not have
Stop extraction when what is produced；Vacuum breaker is vented, slagged tap while hot, obtains about 390 kilograms of cut in 4- aldehyde radicals-allyl acetonitrile (CFN),
Content >=82% is standby for next unit.
Embodiment 5：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1 or 2 or 3 or 4 or 5, described step (4)
4- aldehyde radicals-allyl acetonitrile (CFN) chlorination is that 900 kilograms of dimethylformamides (DMF) and 900 kilograms of CFN are put into chlorination
In kettle, start chlorination tank stirring and circulating pump, material is cooled to 5 DEG C, open the outlet valve of chlorine cylinder, lead into system
Enter about 650 kilograms of CL2, control material temperature is at 0 DEG C~5 DEG C, until reaction reaches terminal, the material that chlorination is completed heats up naturally
CCC degassing kettles are transferred to after to 5 DEG C of 10 DEG C~l insulations 1 hour, then are incubated 1 hour, decompression degassing, end temperature≤30 DEG C take off
For cyclization post after depressed beam.
Embodiment 6：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1 or 2 or 3 or 4 or 5 or 6, described step
(5) 4- aldehyde radicals -4,5- dichloro valeronitrile (CCC) cyclisation method is that being pumped into 2000kg TOL into CCC cyclization kettles, (moisture content is less than
0.1%) with half batch of CCC-DMF solution, the stirring of cyclization kettle is started, temperature in kettle is risen into 90 DEG C starts that 350 kilograms of trichlorines are added dropwise
Oxygen phosphorus (POCL3), it is 90 ± 2 DEG C to control temperature, and time for adding is 3.5~4 hours, anti-in 90 ± 2 DEG C of insulations after completion of dropwise addition
Answer 1 hour and start sampling analysis, terminate reaction when CCC contents≤2%, be cooled to 75 DEG C~80 DEG C degree blowings and enter hydrolysis and neutralize
Kettle.
Embodiment 7：
According to embodiment 1 or 2 or 3 or 4 or 5 or described 2-vhloro-5-chloromethylpyridine process for purification, it is characterized in that：Institute
The step of stating (6) hydrolysis, neutralization method are to start the stirring that hydrolysis neutralizes kettle, and material in kettle is cooled into 35 DEG C~45 DEG C, to
1200 kg of water are added dropwise in kettle to be hydrolyzed, the water of lower floor sour water surge tank are put into, upper toluene layer is stayed in kettle, into kettle
Soda ash solution is added dropwise, and measures the pH value of material in time, pH value answers=8, stirring 30 minutes is then proceeded to, repetition measurement pH value reaches will
Ask, then stop stirring, stand 60 minutes and be layered, the moisture of lower floor is entered into neutral water storage tank, toluene is put into CCP- toluene solutions and delayed
Rush tank.
Embodiment 8：
2-vhloro-5-chloromethylpyridine process for purification according to embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7, described step
Suddenly it is to start the de- benzene vacuum pump set of film desolventizing system, point that (7) 2-vhloro-5-chloromethylpyridine (CCMP), which takes off benzene, process for purification,
The dynamic motor for starting CCP thin film evaporators, thin film evaporator is pumped into by the toluene solutions of CCP mono-, it is ensured that CMCP drop temperatures are kept
At 60 DEG C~75 DEG C, the good CCP of precipitation is pumped into bis- de- benzene kettles of CCMP.Precipitation is depressurized to finally, it is desirable to which kettle temperature is no more than 95
DEG C, sampling analysis toluene level≤5% terminates, and cools standby to 60 DEG C~70 DEG C blowing meterings, takes out thick CCMP550 kilograms
Enter in 500L distillation stills.Open jacket steam heating, required according to finished product content, before accurately cutting, in evaporate, when kettle temperature reaches 160
DEG C~165 DEG C, when now being come out without rear fraction, jacket steam valve is closed, begin to rehearse slag air-introduced machine, be slowly opened into and all open sufficient put
After the empty valve several seconds, the rapid deslagging of fully open bottom valve, while hot goes out slag in kettle to the greatest extent immediately.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of 2-vhloro-5-chloromethylpyridine process for purification, it is characterized in that：This method comprises the following steps：
（1）Dicyclopentadiene（DCP）Cracking；
（2）5- ENBs（CN）Synthesis；
（3）- 2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene（CCN）Addition, de- benzene, cracking；
（4）4- aldehyde radicals-allyl acetonitrile（CFN）Chlorination；
（5）4- aldehyde radical -4,5- dichloro valeronitriles（CCC）Cyclization；
（6）Hydrolysis, neutralization；
（7）2-vhloro-5-chloromethylpyridine（CCMP）Take off benzene, refine.
2. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（1）It is bicyclic
Pentadiene（DCP）Cleavage method is, when the oil outlet temperature of vaporizes kettle and thin film evaporator reaches 240 degree, opens DCP chargings
Pump, opens thin film evaporator and vaporizes kettle stirring, is fed to cracking system, there is cyclopentadiene（CP）During extraction, sampling in time
Analysis gained CP contents, content requirement control tower top top temperature for 50 DEG C ± 5 DEG C more than 97%, adopt outlet temperature be -5 DEG C~+
10 DEG C, the CP of collection is standby for next unit.
3. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（2）5- drops
Bornylene（CN）Synthetic method is, by 750 kilograms of methacrylaldehyde for entering in CN synthesis reactors, to open the recirculated water of synthesis reactor cooling coil
Valve is passed in and out, starts synthesis reactor stirring, 870 kilograms of CP is slowly added dropwise into kettle, by dropping temperature control at 40 DEG C~45 DEG C, drop
Plus terminate, continuation insulation reaction sampling analysis after 5 ~ 6 hours, methacrylaldehyde≤0.5% is reaction end, reacts to obtain 5- ENBs
（CN）It is standby for next unit.
4. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（3）Ring
- 2 β of hept- 2- aldehyde-propionitrile -5- alkene（CCN）Addition, de- benzene, cleavage method are, by 3000 kilograms of toluene（TOL）With 380 kilogram third
Alkene nitrile（AN）For entering in addition kettle, start reactor stirring, be warming up to 25 DEG C, add 20 kilograms of tert-butyl alcohols and 8 kilograms of hydrogen-oxygens
Change and 560 kilograms of CN are added dropwise after potassium into addition kettle, controlling reaction temperature is in 25 DEG C~28 DEG C, the follow-up continuous insulation reaction of completion of dropwise addition
Sampling analysis after 1 hour, CN contents≤1.0%, which reacts, to be terminated, and reacts to obtain -2 β of cycloheptyl -2- aldehyde-propionitrile -5- alkene（CCN）Toluene is molten
Liquid；Start the de- benzene vacuum pump set of film desolventizing system, start the cloth motor of thin film evaporator, open CCN- toluene liquid
Feed pump, feeds to thin film evaporator, opens the heating steam of thin film evaporator, it is ensured that CCN concentrate drop temperatures are maintained at
60 DEG C~85 DEG C；Oilless vertical vacuum pump is opened, CCN concentrates are put into CFN cracking stills（1300 kilograms）, open conduction oil
Import and export valve, starts slow heating, infinite reflux when pushing up temperature to 90 DEG C to the fraction that hits is started, until kettle temperature to 200 DEG C, tower
Stop extraction when what top produce without；Vacuum breaker is vented, slagged tap while hot, obtains 4- aldehyde radicals-allyl acetonitrile（CFN）Middle cut is about
390 kilograms, content >=82% is standby for next unit.
5. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（4）4- aldehyde
Base-allyl acetonitrile（CFN）Chlorination is, by 900 kilograms of dimethylformamides（DMF）With 900 kilograms of CFN input chlorination tanks
In, start chlorination tank stirring and circulating pump, material is cooled to 5 DEG C, open the outlet valve of chlorine cylinder, be passed through into system
About 650 kilograms of CL2, control material temperature is at 0 DEG C~5 DEG C, until reaction reaches terminal, the material that chlorination is completed is warmed naturally to
CCC degassing kettles are transferred to after 5 DEG C of 10 DEG C~l insulations 1 hour, then are incubated 1 hour, decompression degassing, end temperature≤30 DEG C, degassing
For cyclization post after end.
6. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（5）4- aldehyde
Base -4,5- dichloro valeronitrile（CCC）Cyclisation method is to be pumped into 2000kg TOL into CCC cyclization kettles（Moisture content is less than 0.1%）With half
CCC-DMF solution is criticized, starts the stirring of cyclization kettle, temperature in kettle is risen into 90 DEG C starts that 350 kilograms of POCl3s are added dropwise
（POCL3）, it is 90 ± 2 DEG C to control temperature, and time for adding is 3.5~4 hours, small in 90 ± 2 DEG C of insulation reactions 1 after completion of dropwise addition
When start sampling analysis, terminate reaction when CCC contents≤2%, be cooled to 75 DEG C~80 DEG C degree blowings and enter hydrolysis and neutralize kettle.
7. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（6）Water
Solution, neutralization method are to start the stirring that hydrolysis neutralizes kettle, and material in kettle is cooled into 35 DEG C~45 DEG C, 1200 are added dropwise into kettle
Kg of water is hydrolyzed, and the water of lower floor is put into sour water surge tank, and upper toluene layer is stayed in kettle, soda ash is added dropwise into kettle molten
Liquid, and the pH value of material is measured in time, pH value answers=8, then proceedes to stirring 30 minutes, repetition measurement pH value reaches requirement, then stops stirring
Mix, stand 60 minutes and be layered, the moisture of lower floor is entered into neutral water storage tank, toluene is put into CCP- toluene solution surge tanks.
8. 2-vhloro-5-chloromethylpyridine process for purification according to claim 1, it is characterized in that：Described step（7）2-
Chlorine-5-chloromethyl pyridine（CCMP）De- benzene, process for purification are to start the de- benzene vacuum pump set of film desolventizing system, and crawl starts
The motor of CCP thin film evaporators, is pumped into thin film evaporator, it is ensured that CMCP drop temperatures are maintained at 60 DEG C by the toluene solutions of CCP mono-
~75 DEG C, the good CCP of precipitation is pumped into bis- de- benzene kettles of CCMP, decompression precipitation is to finally, it is desirable to which kettle temperature is no more than 95 DEG C, sampling
Analyze toluene level≤5% to terminate, cool standby to 60 DEG C~70 DEG C blowing meterings, take out thick CCMP550 kilograms and enter 500L
In distillation still, open jacket steam heating, required according to finished product content, before accurately cutting, in evaporate, when kettle temperature reaches 160 DEG C~165
DEG C, when now being come out without rear fraction, jacket steam valve is closed, begin to rehearse slag air-introduced machine, be slowly opened into and all open sufficient atmospheric valve number
After second, the rapid deslagging of fully open bottom valve, while hot goes out slag in kettle to the greatest extent immediately.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689918A (en) * | 2017-11-29 | 2018-10-23 | 山东汇盟生物科技有限公司 | Rectification process of 2-chloro-5-chloromethylpyridine |
| CN110015986A (en) * | 2019-04-29 | 2019-07-16 | 山东汇盟生物科技股份有限公司 | 2-chlorine-2-chloromethyl-4-cyano butyraldehyde cyclization device |
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| CN110015986A (en) * | 2019-04-29 | 2019-07-16 | 山东汇盟生物科技股份有限公司 | 2-chlorine-2-chloromethyl-4-cyano butyraldehyde cyclization device |
| WO2020221147A1 (en) * | 2019-04-29 | 2020-11-05 | 山东汇盟生物科技股份有限公司 | 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization device |
| CN110015986B (en) * | 2019-04-29 | 2024-02-20 | 山东汇盟生物科技股份有限公司 | 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device |
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