CN110015986B - 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device - Google Patents
2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device Download PDFInfo
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- CN110015986B CN110015986B CN201910353013.XA CN201910353013A CN110015986B CN 110015986 B CN110015986 B CN 110015986B CN 201910353013 A CN201910353013 A CN 201910353013A CN 110015986 B CN110015986 B CN 110015986B
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- 238000007363 ring formation reaction Methods 0.000 title claims abstract description 102
- 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 16
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 147
- 230000007062 hydrolysis Effects 0.000 claims abstract description 117
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 70
- 238000003860 storage Methods 0.000 claims abstract description 69
- 238000005406 washing Methods 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000605 extraction Methods 0.000 claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 54
- 238000005191 phase separation Methods 0.000 claims description 43
- 239000002253 acid Substances 0.000 claims description 16
- 238000003809 water extraction Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- 238000010992 reflux Methods 0.000 claims description 11
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 21
- 239000011734 sodium Substances 0.000 description 9
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 8
- SKCNYHLTRZIINA-UHFFFAOYSA-N 2-chloro-5-(chloromethyl)pyridine Chemical compound ClCC1=CC=C(Cl)N=C1 SKCNYHLTRZIINA-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000010865 sewage Substances 0.000 description 5
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- QDECAQIUBBSGKI-UHFFFAOYSA-N 3-(5-formyl-4-bicyclo[2.2.1]hept-2-enyl)propanenitrile Chemical compound C1C2(CCC#N)C(C=O)CC1C=C2 QDECAQIUBBSGKI-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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000005906 Imidacloprid Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- -1 at present Chemical compound 0.000 description 1
- 230000009286 beneficial effect Effects 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
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000007547 defect Effects 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
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003385 ring cleavage reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 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 invention relates to a 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device, which comprises a temporary storage tank I, a temporary storage tank II, a temporary storage tank III, a temporary storage tank IV and Na 2 CO 3 The solution storage tank, the temporary storage tank I and the temporary storage tank II are connected with the mixer I and the condenser I, the cyclization reaction units are connected with the temporary storage tank III, the last-stage cyclization reaction unit is connected with the two-stage hydrolysis unit I, and the last-stage hydrolysis unit I is connected with the hydrolysis unit II; the hydrolysis unit II is sequentially connected with the extraction unit, the neutralization unit, the water washing unit and the desolventizing unit, the extraction unit is connected with the temporary storage tank II, the desolventizing unit is connected with the secondary desolventizing unit, and the secondary desolventizing unit is connected with the tertiary desolventizing unit; the temporary storage tank IV is connected with the two-stage hydrolysis unit I, the water washing unit and the hydrolysis unit, and Na 2 CO 3 The solution storage tank is connected with the neutralization unit. The invention can reduce side reaction, improve product yield, realize continuous feeding and discharging, and save production time.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device.
Background
2-cyanoethyl-5-norvalopenem-2-aldehyde (CCN) is an intermediate for synthesizing 2-chloro-5-chloromethylpyridine, 2-chloro-5-chloromethylpyridine is an important pesticide and medical intermediate, and is an important raw material for synthesizing efficient low-toxicity pesticide imidacloprid, at present, 2-chloro-5-chloromethylpyridine is mostly produced in China by double ring cleavage, cyclopentadiene is cleaved to produce Cyclopentadiene (CP), cyclopentadiene and acrolein are added to produce 5-norbornene-2-formaldehyde (CN), CN and acrylonitrile are added to produce 2-cyanoethyl-5-norbornene-2-aldehyde (CCN), CCN is cleaved to 2-methylene-4-Cyanobutyraldehyde (CFN), CFN is chlorinated to produce 2-chloro-2-chloromethyl-4-cyanobutyraldehyde (CCC), CCC is cyclized to produce 2-chloro-5-chloromethylpyridine, and the sixth step is to cyclize 2-chloro-5-chloromethylpyridine from 2-chloro-2-chloromethyl-4-cyanobutyraldehyde (CCC).
In the prior art, intermittent synthesis and treatment are adopted in the cyclization section, the cyclization reaction is an exothermic reaction, the retention time of materials in a container is long, the polymerization of the materials is indirectly promoted, the generated energy is not timely and effectively dispersed, the side reaction is more, and the yield of the product is not high; meanwhile, intermittent reaction is adopted for hydrolysis, neutralization, water washing and desolventizing, and the delay time of material transferring and feeding is equivalent to reduce the production efficiency, and the incomplete hydrolysis, neutralization and water washing are caused, so that the yield and purity of the product are affected.
Disclosure of Invention
The invention overcomes the defects in the prior art and provides a 2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device.
In order to solve the technical problems, the invention is realized by the following technical scheme: a2-chloro-2-chloromethyl-4-cyano butyraldehyde cyclization device comprises a temporary storage tank I, a temporary storage tank II, a temporary storage tank III, a temporary storage tank IV and Na 2 CO 3 The solution storage tank is characterized in that the temporary storage tank I and the temporary storage tank II are connected with a mixer I, the mixer I is connected with a condenser I, the condenser I is connected with a plurality of annular reaction units, each annular reaction unit is connected with the temporary storage tank III, the annular reaction units at the last stage are respectively connected with two hydrolysis units I, and the hydrolysis units I at the last stage are connected with a hydrolysis unit II; the hydrolysis unit II is connected with the extraction unit, the extraction unit is connected with the temporary storage tank II and the neutralization unit, the neutralization unit is connected with the washing unit, the washing unit is connected with the desolventizing unit and the temporary storage tank IV, the desolventizing unit is connected with the reflux unit and the secondary desolventizing unit, and the secondary desolventizing unit is connected with the tertiary desolventizing unit; the temporary storage tank IV is connected with the two-stage hydrolysis unit I, the temporary storage tank IV is connected with the hydrolysis unit through a condenser VII, and the Na is 2 CO 3 The solution storage tank is connected with the neutralization unit.
As a preferred scheme, the multistage cyclization reaction unit comprises a primary cyclization reaction unit, a secondary cyclization reaction unit, a tertiary cyclization reaction unit, a quaternary cyclization reaction unit, a five-stage cyclization reaction unit, a six-stage cyclization reaction unit, a seven-stage cyclization reaction unit and an eight-stage cyclization reaction unit which are connected in series, each stage of the cyclization reaction unit comprises a cyclization reactor, a reboiler, a mixer, a condenser and a catcher, the cyclization reactors are externally connected with the reboiler and the mixer, the upper part of each cyclization reactor is connected with the condenser, the catcher is connected with each catcher, the last-stage catcher is respectively connected with the two-stage hydrolysis unit I and the three-time desolventizing unit, and each mixer is connected with the temporary storage tank III.
Preferably, the hydrolysis unit I comprises a primary hydrolysis unit I and a secondary hydrolysis unit I, and the primary hydrolysis unit I comprises 1 # Hydrolysis reaction kettle, 1 # The hydrolysis reaction kettle is externally connected with 1 # A cooler, 1 # A discharge hole at the upper part of the hydrolysis reaction kettle is connected with a condenser V, and the condenser V is connected with a catcher; the secondary hydrolysis unit I comprises 2 # Hydrolysis reaction kettle, 2 # The hydrolysis reaction kettle is externally connected with 2 # Cooler, described 2 # A discharge hole at the upper part of the hydrolysis reaction kettle is connected with a condenser VI, and the condenser VI is connected with a cooler I; said 1 # Hydrolysis reaction kettle and 2 # The hydrolysis reaction kettles are connected with a temporary storage tank IV.
Preferably, the hydrolysis unit II comprises a hydrolysis tower feed buffer tank and a hydrolysis tower, wherein the hydrolysis tower feed buffer tank is respectively connected with the hydrolysis tower feed buffer tank and the hydrolysis tower feed buffer tank 2 # The hydrolysis reaction kettle is connected with a hydrolysis tower, and the upper part of the hydrolysis tower is connected with a condenser VII and a toluene washing tower; the top and the bottom of the hydrolysis tower are respectively connected with a hydrolysis tower light phase separation tank and a hydrolysis tower heavy phase separation tank, the hydrolysis tower heavy phase separation tank is respectively connected with a hydrolysis tower light phase separation tank and a hydrolysis tower heavy phase receiving tank, both the hydrolysis tower light phase separation tank and the hydrolysis tower heavy phase separation tank are connected with a hydrolysis tower light phase receiving tank, the hydrolysis tower heavy phase receiving tank is connected with an acid water extraction tower, and the hydrolysis tower light phase receiving tank is connected with a neutralization tower feeding buffer tank.
As a preferred scheme, the extraction unit comprises an acid water extraction tower, wherein the upper part and the lower part of the acid water extraction tower are respectively connected with a tower top phase-splitting tank and a tower bottom phase-splitting tank, and the tower top phase-splitting tank and the tower bottom phase-splitting tank are both connected with a neutralization tower feeding buffer tank; and the feeding port of the acid water extraction tower is connected with a temporary storage tank II.
Preferably, the neutralization unit comprises a catalyst selected from the group consisting of sodium, and a mixture thereof 2 CO 3 The top and the bottom of the neutralization tower are respectively connected with a light component phase separation tank and a heavy component phase separation tank of the neutralization tower, and the light component phase separation tank of the neutralization tower and the heavy component phase separation tank of the neutralization tower are both connected with the neutralization towerThe light component receiving tank is connected with the heavy component receiving tank of the neutralization tower at the bottom of the heavy component phase splitting tank of the neutralization tower, and the light component receiving tank of the neutralization tower is connected with the toluene liquid washing tower.
As a preferable scheme, the water washing unit comprises a toluene liquid water washing tower, the top and the bottom of the toluene liquid water washing tower are respectively connected with a light component phase-splitting tank of the water washing tower and a heavy component phase-splitting tank of the water washing tower, and the light component phase-splitting tank of the water washing tower is connected with a feeding buffer tank of the desolventizing tower.
As a preferable scheme, the desolventizing unit comprises a desolventizing tower, the desolventizing tower is externally connected with a cooler II, the upper part of the desolventizing tower is connected with a desolventizing tower reflux tank, the top of the desolventizing tower is connected with a desolventizing tower condenser, the desolventizing tower condenser is connected with a desolventizing tower catcher, and the desolventizing tower condenser and the desolventizing tower catcher are both connected with the desolventizing tower reflux tank; .
The secondary desolventizing unit comprises a scraper evaporator I and a scraper evaporator II which are connected in series, wherein the scraper evaporator I is connected with the desolventizing tower; the scraper evaporator I and the scraper evaporator II are respectively connected with the scraper evaporator receiving tank I and the scraper evaporator receiving tank II, the top outlets of the scraper evaporator I and the scraper evaporator II are connected with the scraper condenser, the scraper condenser is connected with the scraper catcher, and the scraper condenser and the scraper catcher are connected with the collecting tank; the outlet of the scraper evaporator II is connected with 1 # And (5) forced circulation kettle.
Preferably, the three desolventizing units comprise 1 in series # Forced circulation kettle 2 # Forced circulation kettle and 3 # Forced circulation kettle, 1 # Forced circulation kettle 2 # Forced circulation kettle and 3 # The upper discharge port of the forced circulation kettle is respectively connected with a condenser II, a condenser III and a condenser IV, and the condenser II, the condenser III and the condenser IV are respectively connected with a receiving tank I, a receiving tank II and a receiving tank III.
Compared with the prior art, the invention has the beneficial effects that: the cyclization working section of the invention adopts continuous synthesis and treatment, the system materials react in the container and circulate outside the kettle, the residence time of the materials in the same container is reduced, the polymerization of the materials is directly reduced, the generated energy can be timely and effectively dispersed, the occurrence of side reaction is greatly reduced, and the yield of the product is improved; the invention uses tower type to realize continuous feeding and discharging, which saves production time greatly, and improves production efficiency, hydrolysis, neutralization and water washing more thoroughly, thereby improving product yield and purity.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
In the figure, 101, temporary storage tanks I and 102, temporary storage tanks II and 103, temporary storage tanks III and 104, temporary storage tanks IV and 105, a hydrolysis tower feeding buffer tank 106, a hydrolysis tower light phase separation tank 107, a hydrolysis tower heavy phase separation tank 108, a hydrolysis tower heavy phase receiving tank 109, a hydrolysis tower light phase receiving tank 110, a tower top phase separation tank 111, a tower bottom phase separation tank 112 and Na 2 CO 3 Solution storage tank, 113, neutralization column feed buffer tank, 114, neutralization column light component phase separation tank, 115, neutralization column heavy component phase separation tank, 116, neutralization column heavy component receiving tank, 117, neutralization column light component receiving tank, 118, water wash column light component phase separation tank, 119, water wash column heavy component phase separation tank, 120, desolventizing column feed buffer tank, 121, desolventizing column reflux 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 reactor, 202, 2 # Cyclization reactor, 203, 3 # Cyclization reactors, 204, 4 # Cyclization reactors, 205, 5 # Cyclization reactors, 206, 6 # Cyclization reactors, 207, 7 # Cyclization reactors, 208, 8 # Cyclization reactor, 209, 1 # Hydrolysis reaction kettle, 210, 2 # Hydrolysis reaction kettle, 211, 1 # Forced circulation kettle, 212, 2 # Forced circulation kettles 213 and 3 # Forced circulation kettle, 301, 1 # Catcher, 302, 2 # Catcher, 303, 3 # Catcher, 304, 4 # Traps, 305, 5 # Catcher, 306, 6 # Catcher, 307, 7 # Traps, 308, 8 # The trap, 309, the condenser I, 310, the trap I, 311, the cooler I, 312, the desolventizer condenser, 313, the desolventizer trap, 314, the scraper condenser, 315, the scraper trap, 316, the condenser II, 317, the condenser III, 318, the condenser IV, 319, 1 # Reboiler, 320, 2 # Reboiler, 321, 3 # Reboiler, 322, 4 # Reboiler 323, 5 # Reboiler, 324, 6 # Reboiler 325, 7 # Reboiler, 326, 1 # Cooler 327, 2 # Cooler, 328, 1 # Condenser, 329, 2 # Condenser, 330, 3 # Condensers, 331, 4 # Condensers, 332, 5 # Condensers, 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, acid water extraction tower, 503, neutralization tower, 504, toluene liquid water wash tower, 505, desolventizing tower, 601, scraper evaporator i, 602, scraper evaporator ii.
Detailed Description
The present invention will now be described in further detail with reference to the drawings and detailed description, wherein it is to be understood that the embodiments described are merely some, but not all embodiments of the invention.
As shown in FIG. 1, the 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization device comprises a temporary storage tank I101, a temporary storage tank II 102, a temporary storage tank III 103, a temporary storage tank IV 104 and Na 2 CO 3 Solution storage tank 112, temporary storage tank I101, temporary storage tank II 102 all link to each other with blender I401, blender I401 connects condenser I309, condenser I309 connects multistage cyclization reaction unit, each the cyclization reaction unit all links to each other with temporary storage tank III 103, the last level the two-stage hydrolysis unit I is connected respectively to the cyclization reaction unit, the last oneThe hydrolysis unit I is connected with the hydrolysis unit II; the hydrolysis unit II is connected with the extraction unit, the extraction unit is connected with the temporary storage tank II 102 and the neutralization unit, the neutralization unit is connected with the washing unit, the washing unit is connected with the desolventizing unit and the temporary storage tank IV 104, the desolventizing unit is connected with the reflux unit and the secondary desolventizing unit, and the secondary desolventizing unit is connected with the tertiary desolventizing unit; the temporary storage tank IV 104 is connected with the two-stage hydrolysis units I, the temporary storage tank IV 104 is connected with the hydrolysis units through a condenser VII 328, and the Na is 2 CO 3 A solution reservoir 112 is connected to the neutralization unit.
In one embodiment, the multistage cyclization reaction unit comprises a first-stage cyclization reaction unit, a second-stage cyclization reaction unit, a third-stage cyclization reaction unit, a fourth-stage cyclization reaction unit, a fifth-stage cyclization reaction unit, a sixth-stage cyclization reaction unit, a seventh-stage cyclization reaction unit and an eighth-stage cyclization reaction unit which are connected in series, each stage of the cyclization reaction unit comprises a cyclization reactor, a reboiler, a mixer, a condenser and a catcher, the reactor is externally connected with the reboiler and the mixer, the upper part of the reactor is connected with the condenser, the catcher is connected with the catcher, each catcher is connected with the catcher, the tail gas from each catcher is removed from the tail gas absorbing device, the last-stage catcher is respectively connected with the two-stage hydrolysis unit I and the three-stage desolventizing unit, and each mixer is connected with the temporary storage tank III 103.
In one embodiment, the primary cyclization reaction unit comprises 1 # Cyclization reactor 201, said 1 # The cyclization reactor 201 is externally connected with 1 in series # Reboiler 319 and 1 # Mixer 402, described 1 # The upper discharge port of the cyclization reactor 201 is connected with 1 # Condenser 328, described 1 # The upper outlet of the condenser 328 is connected with 1 # A catcher 301; the secondary cyclization reaction unit comprises 2 # Cyclization reactor 202, 2 # The cyclization reactor 202 is externally connected with 2 in series connection # Reboiler 320 and 2 # Mixer 403, 2 # The upper discharge port of the cyclization reactor 202 is connected with 2 # Condenser 329, 2 # The outlet at the upper part of the condenser 329 is connected with 2 # A catcher 302; the three-stage cyclization reaction unit comprises 3 # A cyclization reactor 203, said 3 # The cyclization reactor 203 is externally connected with 3 in series # Reboiler 321 and 3 # Mixer 404, 3 # The upper discharge port of the cyclization reactor 203 is connected with 3 # Condenser 330, 3 # The upper outlet of the condenser 330 is connected with 3 # A catcher 303; the four-stage cyclization reaction unit comprises 4 # A cyclization reactor 204, said 4 # The cyclization reactor 204 is externally connected with 4 in series connection # Reboiler 322 and 4 # Mixer 405, 4 # 4 discharge ports at the upper part of the cyclization reactor 204 are connected with # Condenser 331, 4 # The upper outlet of the condenser 331 is connected with 4 # A catcher 304; the five-stage cyclization reaction unit comprises 5 # Cyclization reactor 205, said 5 # The cyclization reactor 205 is externally connected with 5 in series # Reboiler 323 and 5 # Mixer 406, 5 # The upper discharge port of the cyclization reactor 205 is connected with 5 # Condenser 332, 5 # The upper outlet of the condenser 332 is connected with 5 # A catcher 305; the six-stage cyclization reaction unit comprises 6 # Cyclization reactor 206, said 6 # The cyclization reactor 206 is externally connected with 6 in series # Reboiler 324 and 6 # Mixer 407, said 6 # The upper discharge port of the cyclization reactor 206 is connected with 6 # Condenser 333, said 6 # The upper outlet of the condenser 333 is connected with 6 # A catcher 306; the seven-stage cyclization reaction unit comprises 7 # Cyclization reactor 207, said 7 # The cyclization reactor 207 is externally connected with 7 in series # Reboiler 325 and 7 # Mixer 408, 7 # 7 is connected with the upper discharge hole of the cyclization reactor 207 # Condenser 334, 7 # The outlet at the upper part of the condenser 334 is connected with 7 # A catcher 307; the eight-stage cyclization reaction unit comprises 8 # Cyclization reactor 208, 8 # The cyclization reactor 208 is externally connected with 8 connected in series # Reboiler 326 and 8 # Mixer 409, 8 # The upper discharge port of the cyclization reactor 208 is connected with 8 # Condenser 335, said 8 # The upper outlet of the condenser 335 is connected with 8 # A catcher 308.
In one embodiment, the hydrolysis unit I comprises a primary hydrolysis unit I and a secondary hydrolysis unit I, the primary hydrolysis unit I comprising 1 # Hydrolysis reaction kettle 209, described 1 # The hydrolysis reaction kettle 209 is externally connected with 1 through a pump # Cooler 326, described 1 # A condenser V336 is connected to a discharge port at the upper part of the hydrolysis reaction kettle 209, and the condenser V336 is connected with a catcher I310; the secondary hydrolysis unit I comprises 2 # Hydrolysis reaction kettle 210, described 2 # The hydrolysis reaction kettle 210 is externally connected with 2 through a pump # Cooler 327, 2 # A discharge port at the upper part of the hydrolysis reaction kettle 210 is connected with a condenser VI 337, and the condenser VI 337 is connected with a cooler I311; the gas from cooler I311 also enters the tail gas absorber; said 1 # Hydrolysis reaction kettles 209 and 2 # The hydrolysis reaction kettles 210 are connected with the temporary storage tank IV 104; 2 # Hydrolysis reactor 210 is connected to hydrolysis column feed buffer tank 105.
In one embodiment, the hydrolysis unit II comprises a hydrolysis tower feed buffer tank 105 and a hydrolysis tower 501, wherein the hydrolysis tower feed buffer tank 105 is connected with the hydrolysis tower 501 through a pump, and the upper part of the hydrolysis tower 501 is connected with a condenser VII 338 and a toluene washing tower 504; the top of the hydrolysis tower 501 is connected with the hydrolysis tower light phase separation tank 106, and the bottom is connected with the hydrolysis tower heavy phase separation tank 107 through a pump; the hydrolysis tower heavy phase split-phase tank 107 is respectively connected with the hydrolysis tower light phase split-phase tank 106 and the hydrolysis tower heavy phase receiving tank 108, the hydrolysis tower light phase split-phase tank 106 and the hydrolysis tower heavy phase split-phase tank 107 are both connected with the hydrolysis tower light phase receiving tank 109, the hydrolysis tower heavy phase receiving tank 108 is connected with the acid water extraction tower 502, and the hydrolysis tower light phase receiving tank 109 is connected with the neutralization tower feeding buffer tank 113.
In one embodiment, the extraction unit comprises an acid water extraction tower 502, wherein the upper part of the acid water extraction tower 502 is connected with a tower top phase separation tank 110, and the lower part of the acid water extraction tower 502 is connected with a tower bottom phase separation tank 111 through a pump; the tower top phase-splitting tank 110 and the tower bottom phase-splitting tank 111 are connected with a neutralization tower feeding buffer tank 113; the feed inlet of the acid water extraction tower 502 is connected with the temporary storage tank II 102; the bottom material of the overhead phase-splitting tank 110 is finally sent to sewage treatment.
In one embodiment, the neutralization unit includes a neutralization unit with Na 2 CO 3 A neutralization tower 503 connected with the solution storage tank 112, wherein the top of the neutralization tower 503 is connected with a neutralization tower light component phase separation tank 114, the bottom of the neutralization tower 503 is connected with a neutralization tower heavy component phase separation tank 115 through a pump, the neutralization tower light component phase separation tank 114 and the neutralization tower heavy component phase separation tank 115 are both connected with a neutralization tower light component receiving tank 117, the bottom of the neutralization tower heavy component phase separation tank 115 is connected with a neutralization tower heavy component receiving tank 116, and the materials at the bottom of the neutralization tower heavy component receiving tank 116 are finally sent to sewage treatment; the neutralization column light component receiving tank 117 is connected to a toluene liquid water washing column 504.
In one embodiment, the water washing unit comprises a toluene liquid water washing tower 504, wherein the top of the toluene liquid water washing tower 504 is connected with a light component phase separation tank 118 of the water washing tower, the bottom of the toluene liquid water washing tower is connected with a heavy component phase separation tank 119 of the water washing tower through a pump, and the material at the bottom of the heavy component phase separation tank 119 of the water washing tower is finally sent to sewage treatment; the water scrubber light component phase separation tank 118 is connected with a desolventizing tower feeding buffer tank 120, and the desolventizing tower feeding buffer tank 120 is connected with a desolventizing tower 505 feeding port.
In one embodiment, the desolventizing unit comprises a desolventizing tower 505, the desolventizing tower 505 is externally connected with a cooler II 339 through a pump, the upper part of the desolventizing tower 505 is connected with a desolventizing tower reflux tank 121, the top part of the desolventizing tower 505 is connected with a desolventizing tower condenser 312, the desolventizing tower condenser 312 is connected with a desolventizing tower catcher 313, and the desolventizing tower condenser 312 and the desolventizing tower catcher 313 are both connected with the desolventizing tower reflux tank 121.
In one embodiment, the secondary desolventizing unit includes a wiped film evaporator I601 and a wiped film evaporator II 602 connected in series, the wiped film evaporator I601 being connected to the desolventizing tower 505; the lower parts of the scraper evaporator I601 and the scraper evaporator II 602 are respectively connected with the scraper evaporator receiving tank I122 and the scraper evaporator receiving tank II 123, and the scraper evaporator receiving tank I122 and the scraper evaporator receiving tank II 123 are respectively connected with the tops of the scraper evaporator I601 and the scraper evaporator II 602 through pumps; outlets at the tops of the scraper evaporator I601 and the scraper evaporator II 602Is connected with a scraper condenser 314, the scraper condenser 314 is connected with a scraper catcher 315, and the scraper condenser 314 and the scraper catcher 315 are connected with the collecting tank 124; the outlet of the scraper evaporator II 602 is connected with 1 # Forced circulation tank 211.
In one embodiment, the triple desolventizing unit includes 1 connected in series by a pump # Forced circulation kettle 211, 2 # Forced circulation kettles 212 and 3 # Forced circulation tank 213, described 1 # Forced circulation kettle 211, 2 # Forced circulation kettles 212 and 3 # The upper discharge port of the forced circulation kettle 213 is respectively connected with a condenser II 316, a condenser III 317 and a condenser IV 318, the condenser II 316, the condenser III 317 and the condenser IV 318 are respectively connected with a receiving tank I125, a receiving tank II 126 and a receiving tank III 127, and gas coming out from the condenser II 316, the condenser III 317 and the condenser IV 318 enters the tail gas absorption device.
The working process is as follows: 2-chloro-2-chloromethyl-4-cyano butyraldehyde (CCC) and anhydrous toluene are fully mixed and dispersed respectively from a temporary storage tank I101 and a temporary storage tank II 102 through a mixer 401, cooled by a condenser I309, enter a cyclization reactor, are fully stirred, and are added with a catalyst from an external circulation reboiler, 1 # The cyclization reactors 201 are sequentially up to 8 # The gas components generated in each cyclization reactor enter an emptying pipeline for tail gas absorption after the action of a condenser and a catcher; after the cyclization is finished, the material enters 1 # Hydrolysis reaction kettles 209 and 2 # The hydrolysis reaction kettle 210 hydrolyzes, gas components generated by hydrolysis enter a vent pipeline for tail gas absorption after the action of a condenser V336, a condenser VI 337, a catcher I310 and a cooler I311, materials enter a hydrolysis tower 501 from bottom to top through a pump by a hydrolysis tower feeding buffer tank 105, tap water enters the hydrolysis tower 501 from top to bottom in a temporary storage tank IV 104 for continuous hydrolysis, after the hydrolysis, the materials are transferred into a hydrolysis tower light phase split-phase tank 106 and a hydrolysis tower heavy phase split-phase tank 107, the hydrolyzed light phase materials enter a neutralization tower feeding buffer tank 113 from a hydrolysis tower light phase receiving tank 109, the hydrolyzed heavy phase components enter an acid water extraction tower 502 from the hydrolysis tower heavy phase receiving tank 108 for primary toluene extraction, and the extracted light phase materials enter an acid water extraction tower 502 for primary toluene extractionFeeding into a buffer tank 113 of the neutralization tower, removing the extracted heavy phase component for wastewater treatment, feeding the extracted light phase material into the neutralization tower 503 from the bottom of the neutralization tower 503 through the buffer tank, and Na 2 CO 3 Solution from Na 2 CO 3 The solution storage tank 112 flows into the tower from the top of the neutralization tower 503, and is subjected to countercurrent mutual washing and neutralization with the extracted materials, the mixed materials enter the neutralization tower light component phase separation tank 114 and the neutralization tower heavy component phase separation tank 115, the light components enter the neutralization tower light component receiving tank 117, the heavy components go to sewage treatment through the neutralization tower heavy component receiving tank 116, the light component materials in the neutralization tower enter the tower from the bottom of the toluene liquid water washing tower 504, tap water enters the tower from the tower top to be subjected to countercurrent mutual washing, after the water washing is finished, the light components are separated again, the light components enter the desolventizing tower 505, the heavy components go to sewage treatment, the light components are desolventized through the desolventizing tower 505, and the desolventized fractions are collected to the desolventizing tower reflux tank 121 for application through the desolventizing tower condenser 312 and the desolventizing tower catcher 313; other materials after desolventizing sequentially enter a scraper evaporator I601 and a scraper evaporator II 602 for secondary desolventizing, the separated fractions of the scraper evaporator I601 and the scraper evaporator II 602 enter a collecting tank 124 after being condensed by a scraper condenser 314 and a scraper catcher 315, tail gas is sent to a tail gas absorbing device for absorption, and other materials after secondary desolventizing enter a tank 1 # Forced circulation kettle 211, 2 # Forced circulation kettle 212, 3 # The forced circulation kettle 213 carries out three-stage desolventizing, the fractions are respectively condensed by a condenser II 316, a condenser III 317 and a condenser IV 318 and are collected and recycled from a receiving tank III 127, tail gas is sent to a tail gas absorbing device for absorption, and other materials after three desolventizing are sent to a rectifying section.
The technical features of the present invention that are not described may be implemented by or by using the prior art, and are not described herein in detail, but the above embodiments are not limited to the embodiments, and the present invention is not limited to the above embodiments, and variations, modifications, additions or substitutions made by those skilled in the art within the spirit and scope of the present invention should also fall within the protection scope of the present invention.
Claims (3)
1. 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization apparatus characterized in that: comprises a temporary storage tank I (101), a temporary storage tank II (102), a temporary storage tank III (103), a temporary storage tank IV (104) and Na 2 CO 3 The solution storage tank (112), the temporary storage tank I (101) and the temporary storage tank II (102) are connected with the mixer I (401), the mixer I (401) is connected with the condenser I (309), the condenser I (309) is connected with the multistage cyclization reaction units, each cyclization reaction unit is connected with the temporary storage tank III (103), the last stage of cyclization reaction units are respectively connected with the two-stage hydrolysis units I, and the last stage of hydrolysis units I are connected with the hydrolysis unit II; the hydrolysis unit II is connected with an extraction unit, the extraction unit is connected with a temporary storage tank II (102) and a neutralization unit, the neutralization unit is connected with a water washing unit, the water washing unit is connected with a desolventizing unit and a temporary storage tank IV (104), the desolventizing unit is connected with a reflux unit and a secondary desolventizing unit, and the secondary desolventizing unit is connected with a tertiary desolventizing unit; the temporary storage tank IV (104) is connected with the two-stage hydrolysis unit I, the temporary storage tank IV (104) is connected with the hydrolysis unit through a condenser VII (328), and the Na is 2 CO 3 A solution storage tank (112) is connected with the neutralization unit; the multistage cyclization reaction units comprise a primary cyclization reaction unit, a secondary cyclization reaction unit, a tertiary cyclization reaction unit, a quaternary cyclization reaction unit, a five-stage cyclization reaction unit, a six-stage cyclization reaction unit, a seven-stage cyclization reaction unit and an eight-stage cyclization reaction unit which are connected in series, wherein each stage of the cyclization reaction unit comprises a cyclization reactor, a reboiler, a mixer, a condenser and a catcher, each cyclization reactor is externally connected with the reboiler and the mixer, the upper part of each cyclization reactor is connected with the condenser, each catcher is connected, the last-stage catcher is respectively connected with the two-stage hydrolysis unit I and the three-time desolventizing unit, and each mixer is connected with the temporary storage tank III (103); the hydrolysis unit I comprises a primary hydrolysis unit I and a secondary hydrolysis unit I, and the primary hydrolysis unit I comprises 1 # Hydrolysis reaction kettle (209), 1 # The hydrolysis reaction kettle (209) is externally connected with 1 # A cooler (326) arranged in a way thatThe 1 # A condenser V (336) is connected to a discharge hole at the upper part of the hydrolysis reaction kettle (209), and the condenser V (336) is connected with a catcher I (310); the secondary hydrolysis unit I comprises 2 # Hydrolysis reaction kettle (210), 2 # The hydrolysis reaction kettle (210) is externally connected with 2 # Cooler (327), 2 # A condenser VI (337) is connected to a discharge port at the upper part of the hydrolysis reaction kettle (210), and the condenser VI (337) is connected with a cooler I (311); said 1 # Hydrolysis reaction kettles (209) and 2 # The hydrolysis reaction kettles (210) are connected with the temporary storage tank IV (104); the hydrolysis unit II comprises a hydrolysis tower feeding buffer tank (105) and a hydrolysis tower (501), wherein the hydrolysis tower feeding buffer tank (105) is respectively connected with the hydrolysis tower feeding buffer tank 2 # The hydrolysis reaction kettle (210) is connected with a hydrolysis tower (501), and the upper part of the hydrolysis tower (501) is connected with a condenser VII (338) and a toluene liquid water scrubber (504); the top and the bottom of the hydrolysis tower (501) are respectively connected with a hydrolysis tower light phase separation tank (106) and a hydrolysis tower heavy phase separation tank (107), the hydrolysis tower heavy phase separation tank (107) is respectively connected with a hydrolysis tower light phase separation tank (106) and a hydrolysis tower heavy phase receiving tank (108), the hydrolysis tower light phase separation tank (106) and the hydrolysis tower heavy phase separation tank (107) are both connected with a hydrolysis tower light phase receiving tank (109), the hydrolysis tower heavy phase receiving tank (108) is connected with an acid water extraction tower (502), and the hydrolysis tower light phase receiving tank (109) is connected with a neutralization tower feeding buffer tank (113); the extraction unit comprises an acid water extraction tower (502), wherein the upper part and the lower part of the acid water extraction tower (502) are respectively connected with a tower top phase-splitting tank (110) and a tower bottom phase-splitting tank (111), and the tower top phase-splitting tank (110) and the tower bottom phase-splitting tank (111) are both connected with a neutralization tower feeding buffer tank (113); the feed inlet of the acid water extraction tower (502) is connected with the temporary storage tank II (102); the neutralization unit comprises a neutralizing unit and Na 2 CO 3 A neutralization tower (503) connected with the solution storage tank (112), wherein the top and the bottom of the neutralization tower (503) are respectively connected with a neutralization tower light component phase separation tank (114) and a neutralization tower heavy component phase separation tank (115), and the neutralization tower light component phase separation tank (114) and the neutralization tower heavy component phase separation tank (115) are connected with each otherAnd a tower light component receiving tank (117), wherein the bottom of the neutralization tower heavy component receiving tank (115) is connected with a neutralization tower heavy component receiving tank (116), and the neutralization tower light component receiving tank (117) is connected with a toluene liquid water washing tower (504); the water washing unit comprises a toluene liquid water washing tower (504), wherein the top and the bottom of the toluene liquid water washing tower (504) are respectively connected with a water washing tower light component phase-splitting tank (118) and a water washing tower heavy component phase-splitting tank (119), the water washing tower light component phase-splitting tank (118) is connected with a desolventizing tower feeding buffer tank (120), and the desolventizing tower feeding buffer tank (120) is connected with a desolventizing tower (505) feeding port; the secondary desolventizing unit comprises a scraper evaporator I (601) and a scraper evaporator II (602) which are connected in series, wherein the scraper evaporator I (601) is connected with a desolventizing tower (505); the scraper evaporator I (601) and the scraper evaporator II (602) are respectively connected with the scraper evaporator receiving tank I (122) and the scraper evaporator receiving tank II (123), the top outlets of the scraper evaporator I (601) and the scraper evaporator II (602) are connected with the scraper condenser (314), and the scraper condenser (314) is connected with the scraper catcher (315); the outlet of the scraper evaporator II (602) is connected with a No. 1 forced circulation kettle (211); the scraper condenser (314) and the scraper catcher (315) are both connected to the collection tank (124).
2. The 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization apparatus of claim 1, wherein: the desolventizing unit comprises a desolventizing tower (505), the desolventizing tower (505) is externally connected with a cooler II (339), the upper part of the desolventizing tower (505) is connected with a desolventizing tower reflux tank (121), the top of the desolventizing tower is connected with a desolventizing tower condenser (312), the desolventizing tower condenser (312) is connected with a desolventizing tower catcher (313), and the desolventizing tower condenser (312) and the desolventizing tower catcher (313) are both connected with the desolventizing tower reflux tank (121).
3. The 2-chloro-2-chloromethyl-4-cyanobutyraldehyde cyclization apparatus of claim 1, wherein: the triple desolventizing unit comprises 1 in series # Forced circulation kettle (211)）、2 # Forced circulation kettles (212) and 3 # Forced circulation tank (213), 1 # Forced circulation kettle (211), 2 # Forced circulation kettles (212) and 3 # The upper discharge port of the forced circulation kettle (213) is respectively connected with a condenser II (316), a condenser III (317) and a condenser IV (318), and the condenser II (316), the condenser III (317) and the condenser IV (318) are respectively connected with a receiving tank I (125), a receiving tank II (126) and a receiving tank III (127).
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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 |
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| CN111269108B (en) * | 2020-01-20 | 2023-08-22 | 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 |
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