CN110015986A - A kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- - Google Patents
A kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- Download PDFInfo
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- CN110015986A CN110015986A CN201910353013.XA CN201910353013A CN110015986A CN 110015986 A CN110015986 A CN 110015986A CN 201910353013 A CN201910353013 A CN 201910353013A CN 110015986 A CN110015986 A CN 110015986A
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- 238000007363 ring formation reaction Methods 0.000 title claims abstract description 112
- MBMUQLSGBUUJLZ-UHFFFAOYSA-N 4-chloro-4-(chloromethyl)-5-oxopentanenitrile Chemical compound ClCC(Cl)(C=O)CCC#N MBMUQLSGBUUJLZ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 230000007062 hydrolysis Effects 0.000 claims abstract description 113
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 113
- 238000001556 precipitation Methods 0.000 claims abstract description 89
- 238000003860 storage Methods 0.000 claims abstract description 58
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 14
- 238000005191 phase separation Methods 0.000 claims description 67
- 230000003472 neutralizing effect Effects 0.000 claims description 49
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 230000003301 hydrolyzing effect Effects 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000000470 constituent Substances 0.000 claims description 23
- 238000003809 water extraction Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- CMQCNTNASCDNGR-UHFFFAOYSA-N toluene;hydrate Chemical compound O.CC1=CC=CC=C1 CMQCNTNASCDNGR-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract 1
- 239000010865 sewage Substances 0.000 description 5
- 238000007792 addition Methods 0.000 description 4
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000003134 recirculating effect Effects 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 1
- -1 2- cyanoethyl -5- Picoline Chemical compound 0.000 description 1
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 1
- CWNRYVQFAMHXLM-UHFFFAOYSA-N 2-formylbutanenitrile Chemical compound CCC(C=O)C#N CWNRYVQFAMHXLM-UHFFFAOYSA-N 0.000 description 1
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 1
- IXMBFEQRFXTDBR-UHFFFAOYSA-N 4-formylpent-4-enenitrile Chemical compound O=CC(=C)CCC#N IXMBFEQRFXTDBR-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005906 Imidacloprid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N anhydrous methyl chloride Natural products ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- AJIBZRIAUXVGQJ-UHFFFAOYSA-N bicyclo[2.2.1]hept-2-ene-5-carbaldehyde Chemical compound C1C2C(C=O)CC1C=C2 AJIBZRIAUXVGQJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 1
- 229940056881 imidacloprid Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization devices of 2-, including temporary storage tank I, temporary storage tank II, temporary storage tank III, temporary storage tank IV and Na2CO3Solution reservoir, temporary storage tank I, temporary storage tank II connect multistage cyclization reaction unit with mixer I, condenser I, each cyclization reaction unit is connected with temporary storage tank III, and afterbody cyclization reaction unit connects two-stage hydrolysis unit I, and afterbody hydrolysis unit I connects hydrolysis unit II；Hydrolysis unit II is sequentially connected extraction cells, neutralisation unit, washing unit, precipitation unit, and extraction cells connect temporary storage tank II, and precipitation unit connects secondary precipitation unit, and secondary precipitation unit is connected with precipitation unit three times；Temporary storage tank IV is connected with two-stage hydrolysis unit I, washing unit, hydrolysis unit, Na2CO3Solution reservoir is connected with neutralisation unit.The present invention can reduce side reaction, improve product yield and be able to achieve continuous feed, discharging, save the production time.
Description
Technical field
The present invention relates to chemical production technical field, in particular to a kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization dress of 2-
It sets.
Background technique
It is the intermediate for synthesizing 2-vhloro-5-chloromethylpyridine, 2 chloro- 5 chlorine that third amylene -2- aldehyde (CCN) drops in 2- cyanoethyl -5-
Picoline is important pesticide and medicine intermediate, is the important source material of synthesizing efficient low-toxin farm chemicals imidacloprid, currently, China
Industrial production 2-vhloro-5-chloromethylpyridine mostly use bicyclic cracking greatly, dicyclopentadiene cracking production cyclopentadiene (CP), ring
Pentadiene and methacrylaldehyde addition generate 5- norbornene -2- formaldehyde (CN), and CN and acrylonitrile addition generate 2- cyanoethyl -5- and drop ice
Piece alkene -2- aldehyde (CCN), CCN are cracked into 2- methylene -4- cyanobutyraldehyde (CFN), and CFN chlorination generates the chloro- 2- chloromethyl -4- of 2-
Cyanobutyraldehyde (CCC), CCC cyclisation generate 2-vhloro-5-chloromethylpyridine, wherein the 6th step is by the chloro- 2- chloromethyl -4- cyanogen of 2-
(CCC) cyclization of base butyraldehyde generates 2-vhloro-5-chloromethylpyridine.
In the prior art, cyclization workshop section uses intermittent synthesis and processing, and cyclization reaction sheet is exothermic reaction, and material is holding
Residence time in device is longer, facilitates the polymerization of material indirectly, and is not in time effectively dispersed the energy of generation,
Side reaction is more, and the yield of product is not high；Hydrolyze, neutralize, washing simultaneously, precipitation is using intermittent reaction, turn that material, feed intake delay
Time equally reduces production efficiency, and cause hydrolysis, neutralize, washing it is incomplete, and then influence the yield of product and pure
Degree.
Summary of the invention
The present invention overcomes deficiencies in the prior art, provide a kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization dress of 2-
It sets.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions: a kind of chloro- 2- chloromethane of 2-
Base -4- cyanobutyraldehyde cyclization device, including temporary storage tank I, temporary storage tank II, temporary storage tank III, temporary storage tank IV and Na2CO3Solution reservoir,
The temporary storage tank I, temporary storage tank II are connected with mixer I, and the mixer I connects condenser I, and the condenser I connects more
Grade cyclization reaction unit, each cyclization reaction unit are connected with temporary storage tank III, cyclization reaction unit described in afterbody point
Not Lian Jie two-stage hydrolysis unit I, hydrolysis unit I described in afterbody connects hydrolysis unit II；The connection of hydrolysis unit II extraction
Take unit, the extraction cells connection temporary storage tank II and neutralisation unit, the neutralisation unit connection washing unit, the washing list
Member connection precipitation unit and temporary storage tank IV, the precipitation unit connection reflux unit and secondary precipitation unit, the secondary precipitation
Unit is connected with precipitation unit three times；The temporary storage tank IV is connected with two-stage hydrolysis unit I, and the temporary storage tank IV passes through condensation
Device VII is connected with hydrolysis unit, the Na2CO3Solution reservoir is connected with neutralisation unit.
Preferably, the multistage cyclization reaction unit includes concatenated level-one cyclization reaction unit, second level cyclization
Reaction member, three-level cyclization reaction member, level Four cyclization reaction unit, Pyatyi cyclization reaction unit, six grades of cyclization reaction units,
Seven grades of cyclization reaction units, eight grades of cyclization reaction units, the cyclization reaction units at different levels include cyclization reaction device, reboiler,
Mixer, condenser and trap, the external reboiler of each cyclization reaction device and mixer, each cyclization reaction device top
It is connected with condenser, the condenser connects trap, and each trap is connected, and afterbody trap is separately connected two
Grade hydrolysis unit I and precipitation unit, each mixer are connected with temporary storage tank III three times.
Preferably, the hydrolysis unit I includes one-stage hydrolysis unit I and second level hydrolysis unit I, the level-one water
Solving unit I includes 1#Hydrolytic reaction pot, described 1#Hydrolytic reaction pot is circumscribed with 1#Cooler, described 1#Hydrolytic reaction pot top goes out
Material mouth is connected with condenser V, and the condenser V connects trap；The second level hydrolysis unit I includes 2#Hydrolytic reaction pot,
Described 2#Hydrolytic reaction pot is circumscribed with 2#Cooler, described 2#Hydrolytic reaction pot upper part discharge port is connected with condenser VI, described cold
Condenser VI connects cooler I；Described 1#Hydrolytic reaction pot and 2#Hydrolytic reaction pot is connected with temporary storage tank IV.
Preferably, the hydrolysis unit II include hydrolysis tower feed surge tank and hydrolysis tower, the hydrolysis tower into
Expect surge tank respectively with 2#Hydrolytic reaction pot is connected with hydrolysis tower, the hydrolysis tower top connection condenser VII and toluene washing
Tower；Hydrolysis tower light phase phase separation tank and hydrolysis tower heavy phase phase separation tank, the hydrolysis are separately connected at the top and bottom of the hydrolysis tower
Tower heavy phase phase separation tank is separately connected hydrolysis tower light phase phase separation tank and hydrolysis tower heavy phase receiving tank, the hydrolysis tower light phase phase separation tank and
Hydrolysis tower heavy phase phase separation tank is connected with hydrolysis tower light phase receiving tank, and the hydrolysis tower heavy phase receiving tank connects sour water extraction tower,
The hydrolysis tower light phase receiving tank connects neutralizing tower feed surge tank.
Preferably, the extraction cells include sour water extraction tower, sour water extraction tower upper and lower part difference
Connection tower top phase separation tank and tower bottom phase separation tank, the tower top phase separation tank and tower bottom phase separation tank are all connected with neutralizing tower feed surge tank；
The sour water extraction tower feed inlet is connected with temporary storage tank II.
Preferably, the neutralisation unit includes and Na2CO3The connected neutralizing tower of solution reservoir, the neutralization tower top
Portion and bottom are separately connected neutralizing tower light component phase separation tank and neutralizing tower heavy constituent phase separation tank, the neutralizing tower light component phase separation tank
Neutralizing tower light component receiving tank is all connected with neutralizing tower heavy constituent phase separation tank, in the neutralizing tower heavy constituent split-phase pot bottom connection
With tower heavy constituent receiving tank, the neutralizing tower light component receiving tank connects toluene liquid water scrubber.
Preferably, the washing unit includes toluene liquid water scrubber, the top and bottom of the toluene liquid water scrubber
Portion is separately connected water scrubber light component phase separation tank and water scrubber heavy constituent phase separation tank, and the water scrubber light component phase separation tank connection is de-
Molten tower feed surge tank.
Preferably, the precipitation unit includes precipitation tower, and the precipitation tower is circumscribed with cooler II, the precipitation
Tower top is connected with precipitation tower return tank, and top is connected with precipitation tower condenser, and the precipitation tower condenser connection precipitation tower is caught
Storage, the precipitation tower condenser and precipitation tower trap are connected with precipitation tower return tank；.
Preferably, the secondary precipitation unit includes concatenated scraper evaporator I and scraper evaporator II, described
Scraper evaporator I is connected with precipitation tower；The scraper evaporator I and scraper evaporator II respectively with scraper evaporator receiving tank I
It is connected with scraper evaporator receiving tank II, the scraper evaporator I and II top exit of scraper evaporator are and scraper condenser
It is connected, the scraper condenser connects scraper plate trap, and the scraper condenser and scraper plate trap are connected with collecting tank；Institute
State the outlet of scraper evaporator II connection 1#Forced circulation kettle.
Preferably, the unit of precipitation three times includes concatenated 1#Forced circulation kettle, 2#Forced circulation kettle and 3#By force
Recirculating still processed, described 1#Forced circulation kettle, 2#Forced circulation kettle and 3#Forced circulation kettle upper part discharge port is connected separately with condenser
II, condenser III and condenser IV, the condenser II, condenser III and condenser IV are separately connected receiving tank I, receiving tank II
With receiving tank III.
Compared with prior art, the beneficial effects of the present invention are: cyclization workshop section of the present invention is synthesized and handled using continous way,
System material is reacted in container and via kettle outer circulation, reduces residence time of the material in same container, directly drop
The low polymerization of material, and can timely and effectively be dispersed the energy of generation, the generation of side reaction is greatly reduced, is mentioned
The high yield of product；Hydrolysis of the invention, extraction, neutralization, washing, precipitation are using tower, it can be achieved that continuous feed, go out
Material, dramatically saves the production time, while improving production efficiency, and what is hydrolyzed, neutralize, washing is more thorough, to improve
The yield and purity of product.
Detailed description of the invention
Fig. 1 is overall structure diagram of the invention.
In figure, 101, temporary storage tank I, 102, temporary storage tank II, 103, temporary storage tank III, 104, temporary storage tank IV, 105, hydrolysis tower into
Material surge tank, 106, hydrolysis tower light phase phase separation tank, 107, hydrolysis tower heavy phase phase separation tank, 108, hydrolysis tower heavy phase receiving tank, 109,
Hydrolysis tower light phase receiving tank, 110, tower top phase separation tank, 111, tower bottom phase separation tank, 112, Na2CO3Solution reservoir, 113, neutralizing tower
Feed surge tank, 114, neutralizing tower light component phase separation tank, 115, neutralizing tower heavy constituent phase separation tank, 116, the reception of neutralizing tower heavy constituent
Tank, 117, neutralizing tower light component receiving tank, 118, water scrubber light component phase separation tank, 119, water scrubber heavy constituent phase separation tank, 120,
Precipitation tower feed surge tank, 121, precipitation tower return tank, 122, scraper evaporator receiving tank I, 123, scraper evaporator receiving tank
II, 124, collecting tank, 125, receiving tank I, 126, receiving tank II, 127, receiving tank III, 201,1#Cyclization reaction device, 202,2#Ring
Conjunction reactor, 203,3#Cyclization reaction device, 204,4#Cyclization reaction device, 205,5#Cyclization reaction device, 206,6#Cyclization reaction device,
207、7#Cyclization reaction device, 208,8#Cyclization reaction device, 209,1#Hydrolytic reaction pot, 210,2#Hydrolytic reaction pot, 211,1#It forces
Recirculating still, 212,2#Forced circulation kettle, 213,3#Forced circulation kettle, 301,1#Trap, 302,2#Trap, 303,3#Trapping
Device, 304,4#Trap, 305,5#Trap, 306,6#Trap, 307,7#Trap, 308,8#Trap, 309, condenser
I, 310, trap I, 311, cooler I, 312, precipitation tower condenser, 313, precipitation tower trap, 314, scraper condenser,
315, scraper plate trap, 316, condenser II, 317, condenser III, 318, condenser IV, 319,1#Reboiler, 320,2#It boils again
Device, 321,3#Reboiler, 322,4#Reboiler, 323,5#Reboiler, 324,6#Reboiler, 325,7#Reboiler, 326,1#It is cooling
Device, 327,2#Cooler, 328,1#Condenser, 329,2#Condenser, 330,3#Condenser, 331,4#Condenser, 332,5#Condensation
Device, 333,6#Condenser, 334,7#Condenser, 335,8#Condenser, 336, condenser V, 337, condenser VI, 338, condenser
VII, 339, cooler II, 401, mixer I, 402, mixer II, 403, mixer III, 404, mixer IV, 405, mixer
V, 406, mixer VI, 407, mixer VII, 408, mixer VIII, 501, hydrolysis tower, 502, sour water extraction tower, 503, neutralization
Tower, 504, toluene liquid water scrubber, 505, precipitation tower, 601, scraper evaporator I, 602, scraper evaporator II.
Specific embodiment
Present invention is further described in detail with specific embodiment with reference to the accompanying drawing, it is clear that described implementation
Example is only a part of the embodiments of the present invention, rather than whole embodiments.
As shown in Figure 1, a kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2-, including temporary storage tank I 101, temporary storage tank
II 102, temporary storage tank III 103, temporary storage tank IV 104 and Na2CO3Solution reservoir 112, the temporary storage tank I 101, temporary storage tank II 102 are equal
It is connected with mixer I 401, the mixer I 401 connects condenser I 309, and the condenser I 309 connects multistage cyclization reaction
Unit, each cyclization reaction unit are connected with temporary storage tank III 103, and cyclization reaction unit described in afterbody is separately connected two
Grade hydrolysis unit I, hydrolysis unit I described in afterbody connect hydrolysis unit II；The hydrolysis unit II connects extraction cells, institute
State extraction cells connection temporary storage tank II 102 and neutralisation unit, the neutralisation unit connection washing unit, the washing unit connection
Precipitation unit and temporary storage tank IV 104, the precipitation unit connection reflux unit and secondary precipitation unit, the secondary precipitation unit
It is connected with precipitation unit three times；The temporary storage tank IV 104 is connected with two-stage hydrolysis unit I, and the temporary storage tank IV 104 passes through cold
Condenser VII 328 is connected with hydrolysis unit, the Na2CO3Solution reservoir 112 is connected with neutralisation unit.
In one embodiment, the multistage cyclization reaction unit includes concatenated level-one cyclization reaction unit, two-stage ring
Close reaction member, three-level cyclization reaction member, level Four cyclization reaction unit, Pyatyi cyclization reaction unit, six grades of cyclization reaction lists
Member, seven grades of cyclization reaction units, eight grades of cyclization reaction units, the cyclization reaction units at different levels include cyclization reaction device, boil again
Device, mixer, condenser and trap, the external reboiler of the reactor and mixer, the reactor top are connected with cold
Condenser, the condenser connect trap, and each trap is connected, and the gas come out from each trap goes tail gas absorption to fill
Set, afterbody trap is separately connected two-stage hydrolysis unit I and three times precipitation unit, each mixer with temporary storage tank III
103 are connected.
In one embodiment, the level-one cyclization reaction unit includes 1#Cyclization reaction device 201, described 1#Cyclization reaction
Device 201 is circumscribed with concatenated 1#Reboiler 319 and 1#Mixer 402, described 1#201 upper part discharge port of cyclization reaction device is connected with
1#Condenser 328, described 1#328 upper outlet of condenser is connected with 1#Trap 301；The second level cyclization reaction member includes
2#Cyclization reaction device 202, described 2#Cyclization reaction device 202 is circumscribed with concatenated 2#Reboiler 320 and 2#Mixer 403, described 2#
202 upper part discharge port of cyclization reaction device is connected with 2#Condenser 329, described 2#329 upper outlet of condenser is connected with 2#Trap
302；The three-level cyclization reaction member includes 3#Cyclization reaction device 203, described 3#Cyclization reaction device 203 is circumscribed with concatenated 3#
Reboiler 321 and 3#Mixer 404, described 3#203 upper part discharge port of cyclization reaction device is connected with 3#Condenser 330, described 3#It is cold
330 upper outlet of condenser is connected with 3#Trap 303；The level Four cyclization reaction unit includes 4#Cyclization reaction device 204, it is described
4#Cyclization reaction device 204 is circumscribed with concatenated 4#Reboiler 322 and 4#Mixer 405, described 4#204 top of cyclization reaction device goes out
Material mouth is connected with 4#Condenser 331, described 4#331 upper outlet of condenser is connected with 4#Trap 304；The Pyatyi cyclization is anti-
Answering unit includes 5#Cyclization reaction device 205, described 5#Cyclization reaction device 205 is circumscribed with concatenated 5#Reboiler 323 and 5#Mixer
406, described 5#205 upper part discharge port of cyclization reaction device is connected with 5#Condenser 332, described 5#The connection of 332 upper outlet of condenser
Have 5#Trap 305；Six grades of cyclization reaction units include 6#Cyclization reaction device 206, described 6#Cyclization reaction device 206 is external
Have concatenated 6#Reboiler 324 and 6#Mixer 407, described 6#206 upper part discharge port of cyclization reaction device is connected with 6#Condenser
333, described 6#333 upper outlet of condenser is connected with 6#Trap 306；Seven grades of cyclization reaction units include 7#Cyclization is anti-
Answer device 207, described 7#Cyclization reaction device 207 is circumscribed with concatenated 7#Reboiler 325 and 7#Mixer 408, described 7#Cyclization reaction
207 upper part discharge port of device is connected with 7#Condenser 334, described 7#334 upper outlet of condenser is connected with 7#Trap 307；It is described
Eight grades of cyclization reaction units include 8#Cyclization reaction device 208, described 8#Cyclization reaction device 208 is circumscribed with concatenated 8#Reboiler 326
With 8#Mixer 409, described 8#208 upper part discharge port of cyclization reaction device is connected with 8#Condenser 335, described 8#On condenser 335
Portion outlet is connected with 8#Trap 308.
In one embodiment, the hydrolysis unit I includes one-stage hydrolysis unit I and second level hydrolysis unit I, the level-one
Hydrolysis unit I includes 1#Hydrolytic reaction pot 209, described 1#Hydrolytic reaction pot 209 is circumscribed with 1 by pump#Cooler 326, described 1#
209 upper part discharge port of hydrolytic reaction pot is connected with condenser V 336, and the condenser V 336 connects trap I 310；Described two
Grade hydrolysis unit I includes 2#Hydrolytic reaction pot 210, described 2#Hydrolytic reaction pot 210 is circumscribed with 2 by pump#Cooler 327, it is described
2#210 upper part discharge port of hydrolytic reaction pot is connected with condenser VI 337, and the condenser VI 337 connects cooler I 311；From cold
But the gas that device I 311 comes out also enters device for absorbing tail gas；Described 1#Hydrolytic reaction pot 209 and 2#Hydrolytic reaction pot 210 with
Temporary storage tank IV 104 is connected；2#Hydrolytic reaction pot 210 connects hydrolysis tower feed surge tank 105.
In one embodiment, the hydrolysis unit II includes hydrolysis tower feed surge tank 105 and hydrolysis tower 501, described
Hydrolysis tower feed surge tank 105 is connected by pump with hydrolysis tower 501,501 top of the hydrolysis tower connection condenser VII 338 and first
Benzene water scrubber 504；The top of the hydrolysis tower 501 connects hydrolysis tower light phase phase separation tank 106, and bottom passes through pump connection hydrolysis tower weight
Phase phase separation tank 107；The hydrolysis tower heavy phase phase separation tank 107 is separately connected hydrolysis tower light phase phase separation tank 106 and hydrolysis tower heavy phase connects
Closed cans 108, the hydrolysis tower light phase phase separation tank 106 and hydrolysis tower heavy phase phase separation tank 107 with 109 phase of hydrolysis tower light phase receiving tank
Even, the hydrolysis tower heavy phase receiving tank 108 connects sour water extraction tower 502, and the hydrolysis tower light phase receiving tank 109 connects neutralizing tower
Feed surge tank 113.
In one embodiment, the extraction cells include sour water extraction tower 502, and 502 top of sour water extraction tower connects
Tower top phase separation tank 110 is connect, lower part passes through pump connection tower bottom phase separation tank 111；The tower top phase separation tank 110 and tower bottom phase separation tank 111
It is all connected with neutralizing tower feed surge tank 113；502 feed inlet of sour water extraction tower is connected with temporary storage tank II 102；Tower top phase separation tank
110 bottoms materials are ultimately destined for sewage treatment.
In one embodiment, the neutralisation unit includes and Na2CO3The connected neutralizing tower 503 of solution reservoir 112, it is described
Neutralizing tower light component phase separation tank 114 is connected at the top of neutralizing tower 503, bottom passes through pump connection neutralizing tower heavy constituent phase separation tank 115, institute
It states neutralizing tower light component phase separation tank 114 and neutralizing tower heavy constituent phase separation tank 115 is all connected with neutralizing tower light component receiving tank 117, institute
State 115 bottom of neutralizing tower heavy constituent phase separation tank connection neutralizing tower heavy constituent receiving tank 116,116 bottom of neutralizing tower heavy constituent receiving tank
The material in portion is ultimately destined for sewage treatment；The neutralizing tower light component receiving tank 117 connects toluene liquid water scrubber 504.
In one embodiment, the washing unit includes toluene liquid water scrubber 504, the toluene liquid water scrubber 504
Top connects water scrubber light component phase separation tank 118, and bottom passes through pump connection water scrubber heavy constituent phase separation tank 119, water scrubber recombination
The material of point 119 bottom of phase separation tank is ultimately destined for sewage treatment；The water scrubber light component phase separation tank 118 connects the charging of precipitation tower
Surge tank 120, the precipitation tower feed surge tank 120 are connected with 505 feed inlet of precipitation tower.
In one embodiment, the precipitation unit includes precipitation tower 505, and the precipitation tower 505 is circumscribed with cold by pump
But device II 339,505 top of precipitation tower are connected with precipitation tower return tank 121, and top is connected with precipitation tower condenser 312, institute
State precipitation tower condenser 312 and connect precipitation tower trap 313, the precipitation tower condenser 312 and precipitation tower trap 313 with
Precipitation tower return tank 121 is connected.
In one embodiment, the secondary precipitation unit includes concatenated scraper evaporator I 601 and scraper evaporator II
602, the scraper evaporator I 601 is connected with precipitation tower 505；II 602 lower part of the scraper evaporator I 601 and scraper evaporator
It is connected respectively with scraper evaporator receiving tank I 122 and scraper evaporator receiving tank II 123, I 122 He of scraper evaporator receiving tank
Scraper evaporator receiving tank II 123 is connected with scraper evaporator I 601 and II 602 top of scraper evaporator by pump again respectively；Institute
It states scraper evaporator I 601 and II 602 top exit of scraper evaporator is connected with scraper condenser 314, the scraper condenser
314 connection scraper plate traps 315, the scraper condenser 314 and scraper plate trap 315 are connected with collecting tank 124；It is described to scrape
The outlet of plate evaporator II 602 connection 1#Forced circulation kettle 211.
In one embodiment, the unit of precipitation three times includes by pumping be connected in series 1#Forced circulation kettle 211,2#By force
Recirculating still 212 and 3 processed#Forced circulation kettle 213, described 1#Forced circulation kettle 211,2#Forced circulation kettle 212 and 3#Forced circulation kettle
213 upper part discharge ports are connected separately with condenser II 316, condenser III 317 and condenser IV 318, the condenser II 316,
Condenser III 317 and condenser IV 318 are separately connected receiving tank I 125, receiving tank II 126 and receiving tank III 127, from condenser
II 316, the gas that condenser III 317 and condenser IV 318 come out enters device for absorbing tail gas.
The course of work is as follows: the chloro- 2- chloromethyl -4- cyanobutyraldehyde (CCC) of 2-, dry toluene are respectively from I 101 and of temporary storage tank
Temporary storage tank II 102 is sufficiently mixed dispersion via mixer 401, enters cyclization reaction device after condenser I 309 is cooling, sufficiently stirs
It mixes, the addition catalyst from outer circulation reboiler, 1#Cyclization reaction device 201 is sequentially into 8#Cyclization reaction device, in each cyclization reaction device
It generates after gas componant is acted on via condenser, trap and enters exhausting pipeline tail gas absorption；After cyclization, material enters 1#
Hydrolytic reaction pot 209 and 2#Hydrolytic reaction pot 210 hydrolyzes, and hydrolysis generates gas componant via condenser V 336, condenser VI
337, trap I 310, cooler I 311 enter exhausting pipeline progress tail gas absorption after acting on, and material feeds slow via hydrolysis tower
It rushes tank 105 and hydrolysis tower 501 is entered by pump from bottom to top, tap water enters from top to bottom from the tap water in temporary storage tank IV 104
Hydrolysis tower 501 continues to hydrolyze, and material is transferred to hydrolysis tower light phase phase separation tank 106 and hydrolysis tower heavy phase phase separation tank 107 after hydrolysis,
Light phase material after hydrolysis enters neutralizing tower feed surge tank 113 from hydrolysis tower light phase receiving tank 109, the heavy phase component after hydrolysis
Enter sour water extraction tower 502 from hydrolysis tower heavy phase receiving tank 108 to extract with a toluene, the light phase material of extraction enters neutralizing tower
Feed surge tank 113, the heavy phase component of extraction go wastewater treatment, and light phase material extracted is via surge tank self-neutralization tower 503
Bottom enter neutralizing tower 503, Na2CO3Solution is from Na2CO3Solution reservoir 112 at the top of neutralizing tower 503 by flowing into tower, with extraction
Material adverse current after taking mutually washes neutralization, and mixed material enters neutralizing tower light component phase separation tank 114 and neutralizing tower heavy constituent phase separation tank
115, light phase component enters neutralizing tower light component receiving tank 117, and heavy constituent goes to sewage via neutralizing tower heavy constituent receiving tank 116
It handling, light component material enters in tower from 504 bottom of toluene liquid water scrubber in neutralizing tower, and tap water enters in tower from tower top, into
Row adverse current is mutually washed, and after washing, separates weight component again, and light component enters precipitation tower 505, and heavy constituent goes to sewage treatment,
Light component via 505 precipitation of precipitation tower, deviate from fraction and pass through precipitation tower condenser 312, precipitation tower trap 313 by precipitation tower 505,
It collects to precipitation tower return tank 121 and applies；Unclassified stores after precipitation sequentially enters scraper evaporator I 601 and scraper evaporator
II 602 2 precipitations, scraper evaporator I 601 and scraper evaporator II 602 deviate from fraction and pass through scraper condenser 314 and scraper plate
Trap 315 enters collecting tank 124 after condensing, and tail gas is gone to device for absorbing tail gas and absorbed, other objects after secondary precipitation
Material enters 1#Forced circulation kettle 211,2#Forced circulation kettle 212,3#Forced circulation kettle 213 carries out three-level precipitation, and fraction is respectively through cold
Condenser II 316, condenser III 317, the condensation of condenser IV 318 collect recovery from receiving tank III 127, and tail gas goes to tail gas suction
Receiving apparatus is absorbed, and the unclassified stores after precipitation goes to rectification section three times.
Technical characteristic of the present invention without description can realize that details are not described herein by or using the prior art, certainly,
Above-mentioned specific embodiment is not limitation of the present invention, and the present invention is also not limited to above-mentioned specific embodiment, this skill
The variations, modifications, additions or substitutions that the those of ordinary skill in art field is made within the essential scope of the present invention should also be fallen into
In protection scope of the present invention.
Claims (10)
1. a kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2-, it is characterised in that: including temporary storage tank I (101), temporary storage tank
II (102), temporary storage tank III (103), temporary storage tank IV (104) and Na2CO3Solution reservoir (112), the temporary storage tank I (101) are kept in
Tank II (102) is connected with mixer I (401), and the mixer I (401) connects condenser I (309), the condenser I
(309) multistage cyclization reaction unit is connected, each cyclization reaction unit is connected with temporary storage tank III (103), afterbody institute
It states cyclization reaction unit and is separately connected two-stage hydrolysis unit I, hydrolysis unit I described in afterbody connects hydrolysis unit II；It is described
Hydrolysis unit II connects extraction cells, and extraction cells connection temporary storage tank II (102) and neutralisation unit, the neutralisation unit connect
Water receiving washes unit, the washing unit connection precipitation unit and temporary storage tank IV (104), the precipitation unit connection reflux unit and
Secondary precipitation unit, the secondary precipitation unit are connected with precipitation unit three times；The temporary storage tank IV (104) and two-stage hydrolysis are single
Member I is connected, and the temporary storage tank IV (104) is connected by condenser VII (328) with hydrolysis unit, the Na2CO3Solution reservoir
(112) it is connected with neutralisation unit.
2. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the multistage
Cyclization reaction unit includes concatenated level-one cyclization reaction unit, second level cyclization reaction member, three-level cyclization reaction member, level Four
Cyclization reaction unit, Pyatyi cyclization reaction unit, six grades of cyclization reaction units, seven grades of cyclization reaction units, eight grades of cyclization reactions
Unit, the cyclization reaction units at different levels include cyclization reaction device, reboiler, mixer, condenser and trap, each ring
The external reboiler of reactor and mixer are closed, cyclization reaction device top is connected with condenser, the condenser connection trapping
Device, each trap are connected, and afterbody trap is separately connected two-stage hydrolysis unit I and three times precipitation unit, each institute
Mixer is stated to be connected with temporary storage tank III (103).
3. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the hydrolysis
Unit I includes one-stage hydrolysis unit I and second level hydrolysis unit I, and the one-stage hydrolysis unit I includes 1#Hydrolytic reaction pot (209),
Described 1#Hydrolytic reaction pot (209) is circumscribed with 1#Cooler (326), described 1#Hydrolytic reaction pot (209) upper part discharge port is connected with
Condenser V (336), the condenser V (336) connect trap I (310)；The second level hydrolysis unit I includes 2#Hydrolysis is anti-
It answers kettle (210), described 2#Hydrolytic reaction pot (210) is circumscribed with 2#Cooler (327), described 2#Hydrolytic reaction pot (210) top goes out
Material mouth is connected with condenser VI (337), and the condenser VI (337) connects cooler I (311)；Described 1#Hydrolytic reaction pot
(209) and 2#Hydrolytic reaction pot (210) is connected with temporary storage tank IV (104).
4. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the hydrolysis
Unit II includes hydrolysis tower feed surge tank (105) and hydrolysis tower (501), the hydrolysis tower feed surge tank (105) respectively with
2#Hydrolytic reaction pot (210) is connected with hydrolysis tower (501), hydrolysis tower (501) top connection condenser VII (338) and toluene
Water scrubber (504)；Hydrolysis tower light phase phase separation tank (106) and hydrolysis tower are separately connected at the top and bottom of the hydrolysis tower (501)
Heavy phase phase separation tank (107), the hydrolysis tower heavy phase phase separation tank (107) are separately connected hydrolysis tower light phase phase separation tank (106) and hydrolysis
Tower heavy phase receiving tank (108), the hydrolysis tower light phase phase separation tank (106) and hydrolysis tower heavy phase phase separation tank (107) are and hydrolysis tower
Light phase receiving tank (109) is connected, and the hydrolysis tower heavy phase receiving tank (108) connects sour water extraction tower (502), and the hydrolysis tower is light
The closed cans that connects (109) connects neutralizing tower feed surge tank (113).
5. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the extraction
Unit includes sour water extraction tower (502), and sour water extraction tower (502) upper and lower part is separately connected tower top phase separation tank (110)
With tower bottom phase separation tank (111), the tower top phase separation tank (110) and tower bottom phase separation tank (111) are all connected with neutralizing tower feed surge tank
(113)；Sour water extraction tower (502) feed inlet is connected with temporary storage tank II (102).
6. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the neutralization
Unit includes and Na2CO3The connected neutralizing tower (503) of solution reservoir (112), neutralizing tower (503) top and bottom connect respectively
Connect neutralizing tower light component phase separation tank (114) and neutralizing tower heavy constituent phase separation tank (115), the neutralizing tower light component phase separation tank
(114) and neutralizing tower heavy constituent phase separation tank (115) is all connected with neutralizing tower light component receiving tank (117), the neutralizing tower heavy constituent
Phase separation tank (115) bottom connects neutralizing tower heavy constituent receiving tank (116), and the neutralizing tower light component receiving tank (117) connects first
Benzene liquid water scrubber (504).
7. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the washing
Unit includes toluene liquid water scrubber (504), is separately connected light group of water scrubber at the top and bottom of the toluene liquid water scrubber (504)
Divide phase separation tank (118) and water scrubber heavy constituent phase separation tank (119), the water scrubber light component phase separation tank (118) connects precipitation tower
Feed surge tank (120), the precipitation tower feed surge tank (120) are connected with precipitation tower (505) feed inlet.
8. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: the precipitation
Unit includes precipitation tower (505), and the precipitation tower (505) is circumscribed with cooler II (339), and precipitation tower (505) top connects
It is connected to precipitation tower return tank (121), top is connected with precipitation tower condenser (312), and precipitation tower condenser (312) connection is de-
Molten tower trap (313), the precipitation tower condenser (312) and precipitation tower trap (313) with precipitation tower return tank (121)
It is connected.
9. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: described secondary
Precipitation unit includes concatenated scraper evaporator I (601) and scraper evaporator II (602), the scraper evaporator I (601) with
Precipitation tower (505) is connected；The scraper evaporator I (601) and scraper evaporator II (602) respectively with scraper evaporator receiving tank
I (122) are connected with scraper evaporator receiving tank II (123), the scraper evaporator I (601) and scraper evaporator II (602) top
Portion outlet is connected with scraper condenser (314), and the scraper condenser (314) connects scraper plate trap (315)；The scraper plate
Evaporator II (602) outlet connection 1# forced circulation kettle (211)；The scraper condenser (314) and scraper plate trap (315) are equal
It is connected with collecting tank (124).
10. the chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- according to claim 1, it is characterised in that: described three
Secondary precipitation unit includes concatenated 1#Forced circulation kettle (211), 2#Forced circulation kettle (212) and 3#Forced circulation kettle (213), institute
State 1#Forced circulation kettle (211), 2#Forced circulation kettle (212) and 3#Forced circulation kettle (213) upper part discharge port is connected separately with cold
Condenser II (316), condenser III (317) and condenser IV (318), the condenser II (316), condenser III (317) and cold
Condenser IV (318) is separately connected receiving tank I (125), receiving tank II (126) and receiving tank III (127).
Priority Applications (2)
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|---|---|---|---|
| CN201910353013.XA CN110015986B (en) | 2019-04-29 | 2019-04-29 | 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device |
| PCT/CN2020/086927 WO2020221147A1 (en) | 2019-04-29 | 2020-04-26 | 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910353013.XA CN110015986B (en) | 2019-04-29 | 2019-04-29 | 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device |
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| CN110015986A true CN110015986A (en) | 2019-07-16 |
| CN110015986B CN110015986B (en) | 2024-02-20 |
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| WO (1) | WO2020221147A1 (en) |
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| CN111269108A (en) * | 2020-01-20 | 2020-06-12 | 泰安渤洋化工科技有限公司 | Continuous hydrolysis device and method for 2,4,6 trimethyl benzoic acid acylation liquid |
| 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 |
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Also Published As
| Publication number | Publication date |
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| WO2020221147A1 (en) | 2020-11-05 |
| CN110015986B (en) | 2024-02-20 |
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