CN104496907B - The method that decompression side line rectification is combined refining imidazoles with drum crystallization continuously - Google Patents
The method that decompression side line rectification is combined refining imidazoles with drum crystallization continuously Download PDFInfo
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- CN104496907B CN104496907B CN201510008087.1A CN201510008087A CN104496907B CN 104496907 B CN104496907 B CN 104496907B CN 201510008087 A CN201510008087 A CN 201510008087A CN 104496907 B CN104496907 B CN 104496907B
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- 150000002460 imidazoles Chemical class 0.000 title claims abstract description 54
- 238000002425 crystallisation Methods 0.000 title claims abstract description 41
- 230000006837 decompression Effects 0.000 title claims abstract description 35
- 230000008025 crystallization Effects 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000007670 refining Methods 0.000 title claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003860 storage Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical group O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229940121375 antifungal agent Drugs 0.000 description 3
- 238000000998 batch distillation Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003429 antifungal agent Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- XMAYWYJOQHXEEK-OZXSUGGESA-N (2R,4S)-ketoconazole Chemical compound C1CN(C(=O)C)CCN1C(C=C1)=CC=C1OC[C@@H]1O[C@@](CN2C=NC=C2)(C=2C(=CC(Cl)=CC=2)Cl)OC1 XMAYWYJOQHXEEK-OZXSUGGESA-N 0.000 description 1
- LEZWWPYKPKIXLL-UHFFFAOYSA-N 1-{2-(4-chlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl}imidazole Chemical compound C1=CC(Cl)=CC=C1COC(C=1C(=CC(Cl)=CC=1)Cl)CN1C=NC=C1 LEZWWPYKPKIXLL-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 206010025421 Macule Diseases 0.000 description 1
- BYBLEWFAAKGYCD-UHFFFAOYSA-N Miconazole Chemical compound ClC1=CC(Cl)=CC=C1COC(C=1C(=CC(Cl)=CC=1)Cl)CN1C=NC=C1 BYBLEWFAAKGYCD-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 239000013556 antirust agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 229960004022 clotrimazole Drugs 0.000 description 1
- VNFPBHJOKIVQEB-UHFFFAOYSA-N clotrimazole Chemical compound ClC1=CC=CC=C1C(N1C=NC=C1)(C=1C=CC=CC=1)C1=CC=CC=C1 VNFPBHJOKIVQEB-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229960003913 econazole Drugs 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 208000030603 inherited susceptibility to asthma Diseases 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000013461 intermediate chemical Substances 0.000 description 1
- 229960004125 ketoconazole Drugs 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229960002509 miconazole Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- -1 vulcanizer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The method that decompression side line rectification is combined refining imidazoles with drum crystallization continuously, adopt continuous intermediate feed mode, raw material squeezes into decompression side line rectifying column still from storage tank, the pressure controlling decompression side line rectifying column is 0.080～0.085Pma, tower top temperature is 65.2～67.7 DEG C, side stream temperature is 123.1～124.9 DEG C, and bottom temperature is 162.2～168.3 DEG C；After separation, overhead components is the water containing trace formaldehyde and Biformyl, and lateral line discharging is containing 96.5% imidazoles fraction, yield more than 98.7%, and bottom is the high boiling point solution such as enrichment Methylimidazole.；Decompression side line rectifying column side run-off mixes with equivalent water, squeezes in continuous crystallisation device, crystallization temperature 20～22 DEG C, and crystal scrapes through scraper, and after funnel extraction, sucking filtration is dried and entered finished pot, obtains more than 99.3% imidazoles, and yield reaches 97.2%.Imidazoles crystal purity of the present invention is high, yield high, simple to operate, energy consumption is low.
Description
Technical field
The present invention relates to a kind of a kind of method for refining imidazoles of medication chemistry method, be specifically related to a kind of method that continuous decompression side line rectification is combined refining imidazoles with drum crystallization.
Background technology
Imidazoles is a kind of important medicine, pesticide intermediate and industrial chemicals, is widely used as the firming agent of epoxy resin, pharmacy antifungal and agricultural chemical insecticide etc..Imidazoles can be used as epoxy curing agent, can improve the mechanical performances such as the bending of goods, stretching, compression, improves the electrical property of insulation, improves the chemical property of chemically-resistant medicament, is widely used in computer, electrical equipment;Printed circuit board and integrated circuit it is used for as the antirust agent of copper;As medical material, for manufacturing antifungal agent, mould resistant, glycopenia therapeutic medicine, artificial plasm, infusorian curative, remedy for bronchial asthma, anti-macule agent etc., imidazoles is the primary raw material preparing antifungal agent miconazole, econazole, ketoconazole and clotrimazole etc.;As pesticide material, for borate compounds synergist, produce insecticide and antibacterial;Additionally, imidazoles also serves as the raw material of urea formaldehyde resin curing agent, photography medicine, binding agent, coating, vulcanizer, antistatic agent etc.;Organic synthesis intermediate.
At present, in imidazoles Refining process, three step gap distillations are adopted to be combined refining imidazoles with kettle type crystallization method, gap distillation and crystallization are all carry out in chuck still, the water of about 98% is removed in the distillation of first step gap, second step batch distillation extracts about 78% imidazoles, and the 3rd step batch distillation extracts about 96% imidazoles, then adopts room temperature crystallization to refine further.Owing to adopting three step batch distillation and crystallizations, distillation and crystallizing cycle are long, constantly regulate vapo(u)rizing temperature and make complicated operation, crystallization process speed is slow, and along with the change of temperature and water temperature, crystallization process is difficult to control to, still-process produces the waste liquid of a large amount of coke-like, and the yield of primary purification imidazoles is only 50%.Obviously, traditional handicraft is for obtaining imidazoles, and production operation is inconvenient, quality stability is poor, yield is low, energy consumption is big.
Summary of the invention
In order to make up the above-mentioned deficiency of existing production, the present invention will provide for a kind of method that continuous decompression side line rectification is combined refining imidazoles with drum crystallization, the industrialization that the method is capable of from imidazoles aqueous solution refining imidazoles crystal.By side line rectification of reducing pressure continuously, obtaining that imidazoles fraction is moisture and trace high boiling component amount stable, again through drum crystallization, imidazoles crystal purity is high, yield is high, and especially this process operation is simple, energy consumption is low.
The scheme completing foregoing invention task is: a kind of continuous decompression side line rectification is combined the method for refining imidazoles with drum crystallization, it is characterised in that step is as follows,
(1). adopting continuous intermediate feed mode, raw material imidazoles aqueous solution squeezes into decompression side line rectifying column still from storage tank 1, begins to warm up when liquid level reaches 1/3 place；
(2). when tower top, bottom temperature start stable, when device reaches infinite reflux, top temperature is 65.2～67.7 DEG C, and side stream temperature is 123.1～124.9 DEG C, and bottom temperature is 162.2～168.3 DEG C；
(3). after separation, overhead components is the water containing trace formaldehyde and Biformyl, and lateral line discharging is for being more than 98.7% containing 96.5% imidazoles fraction, yield, and bottom is the high boiling point solution such as enrichment Methylimidazole.；
(4). decompression side line rectifying column side run-off mixes with the water adding equivalent, and squeezes into rapidly in continuous crystallisation device, and crystallization temperature controls at 20～22 DEG C, and drum rotation speed is 60～65 weeks/h;
(5). crystal scrapes through scraper, enters finished pot through sucking filtration and drying, obtain more than 99.3% imidazoles after funnel extraction, and yield reaches 97.2%.
In above scheme, the content of imidazoles and water respectively 16.4% and 82.12% in described raw material, continuously ratio respectively 0.8269:1,0.1677:1,0.0054:1 of the load of decompression side line rectifying tower top, side line and tower reactor and feedstock amount.
Raw material imidazoles aqueous solution of the present invention is in decompression the 17th piece of plate charging of side line rectifying column continuously, and lateral line discharging is at decompression the 23rd block of plate of side line rectifying column continuously, and the number of plates of side line decompression side line rectifying column is 36 pieces, and inside sets structured packing.
With the refining imidazoles technique of drum crystallization as shown in Figure 1, rectification and crystallization production process condition are as shown in table 1 in decompression side line rectification continuously.
Decompression side line rectification process is as shown in Figure 1 continuously, and device mainly includes condenser 9 and pans 10 at the bottom of raw material storage tank 1, raw material pump 2, effusion meter 3, side line decompression side line rectifying column 4, condenser 5, tower top tank 6, lateral line discharging tank 7, tower underflow gauge 8, tower.In decompression side line distillation process continuously, raw material is squeezed into tower reactor from 1 by pump 2, when liquid level reaches 1/3 place, begins to warm up and treats infinite reflux, and reflux ratio is 2, and top temperature is 65.2～67.7 DEG C, and side stream temperature is 123.1～124.9 DEG C, and bottom temperature is 162.2～168.3 DEG C；Controlling raw material spinner flowmeter with 50.2Kg/h continuous feed, tower top, side line and end load and composition are shown in Table 1.
Drum crystallization device as shown in Figures 2 and 3, raw material storage tank 11, material flow meter 12, drum crystallization device 13, raw material pump 14, crystal storage tank 15, funnel 16, mother liquor holding tank 17.Crystallization raw material storage tank 11 comes from 7 place's imidazoles pregnant solutions, squeezes into 13 through pump.13 internal structures are as it is shown on figure 3, freezing liquid charging aperture 18, drive system 19, rotary drum 20, cooling system 21, freezing liquid outlet 22, feeding spray nozzle 23, doctor blade system 24, frame 25 and mother solution charging tray 26.After raw material enters, drive system 19 drives rotary drum 20 to rotate, sodium chloride freezing liquid enters 18, being released by 22 after cooling system 21, cooling feed liquid, raw material is uniformly sprayed at drum surface by shower nozzle 23, crystal is taken out of by rotary drum, from funnel extraction after doctor blade system 24 scrapes, sucking filtration arrives finished pot 15 after drying, and mother solution charging tray 26 remains mother solution and enters 17 from bottom of device discharge opening.13 place's crystallization temperatures control at 20～22 DEG C, and crystallizer rotary drum 20 rotating speed is 60～65 weeks/h.Decompression side line rectification is combined refining imidazoles crystal with drum crystallization continuously, and separating resulting is as shown in table 2.
The present invention provides a kind of method that continuous decompression side line rectification is combined refining imidazoles with drum crystallization, the industrialization that the method is capable of from imidazoles aqueous solution refining imidazoles crystal.By side line rectification of reducing pressure continuously, obtaining 96.5% imidazoles steady quality, again through drum crystallization, imidazoles crystal purity is high, yield is high, and especially this process operation is simple, energy consumption is low.Reduce pressure under side line rectifying column temperature, input and output material speed, reflux ratio certain condition at continuous lateral line, in imidazoles pregnant solution, imidazole content is disposable can bring up to 96.5%(wt% from 16.4%) more than, yield reaches more than 98.7%, after continuous crystallisation, imidazoles crystal purity is more than 99.3%, and yield is more than 97.2%.
Accompanying drawing explanation
Fig. 1 is continuously decompression side line rectification process figure；
Fig. 2 is continuous crystallisation artwork；
Fig. 3 is crystallization apparatus structure chart.
Detailed description of the invention
Embodiment 1, decompression side line rectification and drum crystallization combine refining imidazoles technique continuously, with reference to Fig. 1, Fig. 2:
(1). adopting continuous intermediate feed mode, raw material imidazoles aqueous solution squeezes into decompression side line rectifying column still from storage tank 1, begins to warm up when liquid level reaches 1/3 place；
(2). when tower top, bottom temperature start stable, when device reaches infinite reflux, top temperature is 65.2～67.7 DEG C, and side stream temperature is 123.1～124.9 DEG C, and bottom temperature is 162.2～168.3 DEG C；
(3). after separation, overhead components is the water containing trace formaldehyde and Biformyl, and lateral line discharging is for being more than 98.7% containing 96.5% imidazoles fraction, yield, and bottom is the high boiling point solution such as enrichment Methylimidazole.；
(4). decompression side line rectifying column side run-off mixes with the water adding equivalent, and squeezes into rapidly in continuous crystallisation device, and crystallization temperature controls at 20～22 DEG C, and drum rotation speed is 60～65 weeks/h;
(5). crystal scrapes through scraper, enters finished pot through sucking filtration and drying, obtain more than 99.3% imidazoles after funnel extraction, and yield reaches 97.2%.
Table 1 reduces pressure side line rectification and drum crystallization process conditions continuously
Table 2 side line rectification of reducing pressure continuously is combined the result of refining imidazoles with drum crystallization
Claims (4)
1. the method that a continuous decompression side line rectification and drum crystallization combine refining imidazoles, it is characterised in that step is as follows,
(1). adopting continuous intermediate feed mode, raw material imidazoles aqueous solution squeezes into decompression side line rectifying column still from storage tank, begins to warm up when liquid level reaches 1/3 place；
(2). when tower top, bottom temperature start stable, when device reaches infinite reflux, top temperature is 65.2～67.7 DEG C, and side stream temperature is 123.1～124.9 DEG C, and bottom temperature is 162.2～168.3 DEG C；
(3). after separation, overhead components is the water containing trace formaldehyde and Biformyl, and lateral line discharging is for being more than 98.7% containing 96.5% imidazoles fraction, yield, and bottom is enrichment Methylimidazole. high boiling point solution；
(4). being mixed by the water that the side run-off that (3) step obtains from decompression side line rectifying column adds equivalent, and squeeze into rapidly in continuous crystallisation device, crystallization temperature controls at 20～22 DEG C, and drum rotation speed is 60～65 weeks/h；
(5). the crystal on cylinder scrapes through scraper, enters finished pot through sucking filtration and drying, obtain more than 99.3% imidazoles finished product after funnel extraction, and yield is 97.2%；
Described decompression side line rectifiying plate number is 36 pieces, and raw material imidazoles aqueous solution is in decompression the 17th piece of plate charging of side line rectifying column, and lateral line discharging is at decompression the 23rd block of plate of side line rectifying column, and inside sets structured packing.
2. the method for the refining imidazoles of continuous decompression side line rectification according to claim 1 and drum crystallization combined techniques, it is characterised in that the content of imidazoles and water respectively 16.4% and 82.12% in described raw material imidazoles aqueous solution.
3. the method for continuous decompression side line rectification according to claim 1 and the refining imidazoles of drum crystallization combined techniques, it is characterized in that, ratio respectively 0.8269:1,0.1677:1,0.0054:1 of the load feedstock amount of described continuous decompression side line rectifying tower top, side line and tower reactor.
4. the method according to the decompression side line rectification continuously one of claim 1-3 Suo Shu and the refining imidazoles of drum crystallization combined techniques, it is characterised in that concrete technology parameter such as table 1:
Table 1 reduces pressure side line rectification and drum crystallization process conditions continuously
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| CN107353926A (en) * | 2017-07-17 | 2017-11-17 | 江苏五洋碳氢科技有限公司 | A kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene |
| CN116675644B (en) * | 2023-06-02 | 2024-07-16 | 临沂大学 | Method for producing imidazole by step interactive cooling crystallization |
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| CN1092644C (en) * | 1999-03-30 | 2002-10-16 | 中国石油化工集团公司 | 4-methylimidazole refining process |
| CN102060863B (en) * | 2010-12-13 | 2012-10-24 | 江苏沿江化工资源开发研究院有限公司 | Method for integrally extracting levamisole hydrochloride by continuous distillation and drum crystallization |
| CN102219699A (en) * | 2011-04-28 | 2011-10-19 | 江苏沿江化工资源开发研究院有限公司 | Method for separating nitroethane and 2-nitropropane by combined process of continuous side distillation and extractive distillation |
| CN103483146B (en) * | 2013-10-15 | 2015-05-27 | 江苏沿江化工资源开发研究院有限公司 | Method for extracting p-tertbutyl benzaldehyde from oxidation reactant of p-tertbutyl methylbenzene through integration of liquid-liquid extraction crystallization and decompression sidetrack rectification |
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