CN109678669A - A kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor - Google Patents
A kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor Download PDFInfo
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- CN109678669A CN109678669A CN201910141230.2A CN201910141230A CN109678669A CN 109678669 A CN109678669 A CN 109678669A CN 201910141230 A CN201910141230 A CN 201910141230A CN 109678669 A CN109678669 A CN 109678669A
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- ethyl acetate
- methanol
- extraction
- rectifying
- rectifying tower
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 764
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 676
- 239000012452 mother liquor Substances 0.000 title claims abstract description 50
- AZZMGZXNTDTSME-JUZDKLSSSA-M cefotaxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 AZZMGZXNTDTSME-JUZDKLSSSA-M 0.000 title claims abstract description 19
- 229960002727 cefotaxime sodium Drugs 0.000 title claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 128
- 239000007788 liquid Substances 0.000 claims abstract description 86
- 239000000203 mixture Substances 0.000 claims abstract description 79
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000003809 water extraction Methods 0.000 claims abstract description 5
- 239000012071 phase Substances 0.000 claims description 112
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 72
- 239000007789 gas Substances 0.000 claims description 65
- 238000000895 extractive distillation Methods 0.000 claims description 53
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- 239000007792 gaseous phase Substances 0.000 claims description 16
- 230000016507 interphase Effects 0.000 claims description 16
- 125000004494 ethyl ester group Chemical group 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 10
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ZTVIKZXZYLEVOL-DGKWVBSXSA-N 2-hydroxy-2-phenylacetic acid [(1R,5S)-8-methyl-8-azabicyclo[3.2.1]octan-3-yl] ester Chemical group C([C@H]1CC[C@@H](C2)N1C)C2OC(=O)C(O)C1=CC=CC=C1 ZTVIKZXZYLEVOL-DGKWVBSXSA-N 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000012797 qualification Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000000284 extract Substances 0.000 description 6
- 230000005484 gravity Effects 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000003808 methanol extraction Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- -1 ethyl ethyl Chemical group 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229930186147 Cephalosporin Natural products 0.000 description 1
- 241000588921 Enterobacteriaceae Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000588770 Proteus mirabilis Species 0.000 description 1
- 241000588767 Proteus vulgaris Species 0.000 description 1
- 241000589516 Pseudomonas Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229960004261 cefotaxime Drugs 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002038 ethyl acetate fraction Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000000401 methanolic extract Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229940007042 proteus vulgaris Drugs 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the devices of a kind of ethyl acetate by Cefotaxime Sodium production mother liquor and separating methanol, including single extraction device, ethyl acetate rectification device, reextraction device and methanol rectifying system；The single extraction device, which is equipped with, is passed through mother liquor with by the liquid inlet of mother liquor isolated first mixture and the second mixture；The different discharge ports of the single extraction device are separately connected the entrance of the ethyl acetate rectification device and the reextraction device, and then ethyl acetate will be obtained after the first mixture rectification, the methanol liquid containing moisture will be obtained after second mixture is defeated plus water extraction and separation；The outlet of the reextraction device connects the entrance of the methanol rectifying system will obtain methanol after the isolated methanol liquid rectifying containing moisture.The device can recycle out the ethyl acetate finished product of 99% or more purity and the methanol finished product of qualification.
Description
Technical field
The present invention relates to chemical products separation technology fields, and in particular to a kind of second for producing Cefotaxime Sodium in mother liquor
The device of acetoacetic ester and separating methanol.
Background technique
Ethyl acetate is also known as ethyl acetate.Pure ethyl acetate is the colorless and transparent liquid with penetrating odor, low
Toxicity, it is pleasantly sweet, it is volatile, to air-sensitive, it can absorb water and divide, so that it is slowly hydrolyzed and is reacted acid, be that a kind of purposes is wide
General fine chemical product has excellent dissolubility, therefore is usually used in the production of chemical intermediate, especially in cephalo-type medicine
As common crystallization solvent in object synthesis.
Methanol (Methano l, dr ied, CH3OH) architecture saturated monohydroxy alcohol the simplest, methanol is widely used,
It is the Organic Chemicals and high-grade fuel on basis.It is mainly used in fine chemistry industry, the fields such as plastics, for manufacturing formaldehyde, vinegar
One of a variety of organic products such as acid, chloromethanes, first ammonia, sulphur dimethyl ester and pesticide, the important source material of medicine.
Cefotaxime is third generation cephalosporin, has a broad antifungal spectrum, to escherichia coli, proteus mirabilis leucocyte, gram
The gram-negative bacterias such as the enterobacteriaceae lactobacteriaceaes such as the primary Pseudomonas of thunder and Salmonella have powerful activity.To proteus vulgaris and citric acid
Bacillus also has good action.Cefotaxime Sodium uses ethyl acetate and methanol in the production of sterile process, in production process
The mother liquor composition of generation is complex, including moisture 8%, ethyl acetate 83%, methanol 8.3%, other solid impurities 0.7%.
For reduce production cost, need in mother liquor ethyl acetate and methanol carry out separation and recycling, reach the secondary quality used
Level, while mitigating the pressure for the treatment of tank, guarantee that sewage after processing reaches national emission standard.Methanol and acetic acid second
Ester azeotropic, 53.9 DEG C of azeotropic point, azeotropic forms methanol 17.6%, ethyl acetate 82.4%.Current rectifying mode is typically just
By the ethyl acetate recycling and reusing in mother liquor, methanol is then used as the interphase of azeotropic composition.
Summary of the invention
It for more efficient recycling ethyl acetate and methanol, increases operation rate, guarantees that quality reaches production and application and requires, this hair
It is bright that the technical problem to be solved is that provide the dress of a kind of ethyl acetate by Cefotaxime Sodium production mother liquor and separating methanol
It sets, using water as extractant, is extracted methanol to aqueous systems, using essence from ethyl acetate system by the method for multitple extraction
Evaporate, extracting rectifying mode by Cefotaxime Sodium produce in mother liquor ethyl acetate and methanol be kept completely separate, while recycle acetic acid
Ethyl ester quality reaches: moisture<0.3%, 10 unit norm color solution of coloration<(Pt-Co), turbidity<0.5#, and ethyl acetate purity>=
99.0%；Methanol quality reaches: moisture < 0.3%, 10 unit norm color solution of coloration < (Pt-Co), turbidity < 0.5#, and methanol is pure
Degree >=99.0%.
The technical scheme to solve the above technical problems is that a kind of acetic acid for producing Cefotaxime Sodium in mother liquor
The device of ethyl ester and separating methanol, including single extraction device, ethyl acetate rectification device, reextraction device and methanol
Rectifier unit；The single extraction device, which is equipped with, is passed through the liquid inlet of mother liquor, and the single extraction device is with by mother liquor
The first mixture and the second mixture are obtained after adding water multitple extraction to separate, first mixture contains small part in mother liquor
Water, most of ethyl acetate and small part methanol contain water, small part acetic acid second most of in mother liquor in second mixture
Ester and most of methanol；The different discharge ports of the single extraction device be separately connected the ethyl acetate rectification device and
The entrance of the reextraction device, and then first mixture is conveyed to the ethyl acetate rectification device and is passed through
Ethyl acetate is obtained after rectification, and second mixture is conveyed to the reextraction device by adding water extraction and separation
The methanol liquid containing moisture is obtained afterwards；The outlet of the reextraction device connects the entrance of the methanol rectifying system to incite somebody to action
The isolated methanol liquid containing moisture is conveyed to the methanol rectifying system by obtaining methanol after rectifying.
The beneficial effects of the present invention are: being slightly soluble in water (15 DEG C, 8.5g/100g) using ethyl acetate, methanol is dissolved in water, second
The acetoacetic ester specific gravity characteristic smaller than water using water as extractant and passes through multitple extraction, by the methanol extraction in mother liquor into water,
Realize the initial gross separation of ethyl acetate and methanol, ethyl acetate extracted recycles out the second of 99% or more purity through rectification
Acetoacetic ester finished product；Aqueous phase dissolved extracted has most methanol and a small amount of ethyl acetate, then passes through by extractant of water
Qualified methanol finished product is finally recycled out in rectifying again after extraction.
Based on the above technical solution, the present invention can also be improved as follows:
Further, the single extraction device include extraction batch can, extractant tank, extraction light phase tank, extraction heavy phase tank and
Three-level extractor；The extraction batch can is equipped with the liquid inlet, and outlet connects the three-level extractor by extraction material pump
Level-one feed inlet；Extraction water is equipped in the extractant tank, outlet connects the three-level extractor by extractant pump
Three-level feed inlet is to provide the extraction water of multitple extraction mother liquor to the three-level extractor and obtain first mixture and institute
State the second mixture；It is light that the three-level light phase discharge port and level-one heavy phase discharge port of the three-level extractor are separately connected the extraction
The entrance of phase tank and the extraction heavy phase tank, and then first mixture and second mixture be conveyed to respectively described
Extract light phase tank and the extraction heavy phase tank.
Using the beneficial effect of above-mentioned further scheme is: using water as extractant and pass through multitple extraction, it will be in mother liquor
Methanol extraction into water, realize ethyl acetate (the first mixture) and methanol (the second mixture) initial gross separation.
Further, the ethyl acetate rectification device includes ethyl acetate rectifying tower reactor, ethyl acetate rectifying column, second
Acetoacetic ester rectifying column first-stage condenser, ethyl acetate rectifying column secondary condenser, ethyl acetate rectifying column cooler, ethyl acetate
Rectifying column water distributing can, ethyl acetate finished product cooler and ethyl acetate tank to be checked；The outlet of the extraction light phase tank passes through light phase
Pump connects the feed inlet of the ethyl acetate rectifying tower reactor so that first mixture is conveyed to the ethyl acetate rectifying column
Kettle is equipped in the ethyl acetate rectifying tower reactor and is passed through steam to heat first mixture and separate from the first mixture
The steam inlet of the ethyl acetate gas of entrapped moisture out；The gaseous phase outlet of the ethyl acetate rectifying tower reactor connects the acetic acid
The gas phase entrance of ethyl ester rectifying column is to be conveyed to the ethyl acetate rectifying column, time liquid for the ethyl acetate gas of entrapped moisture
Mouthful connect the leakage fluid dram of the ethyl acetate rectifying column with after the ethyl acetate gas for isolating entrapped moisture will it is remaining more than
Liquid is conveyed to the ethyl acetate rectifying tower reactor and distills again；The gaseous phase outlet of the ethyl acetate rectifying column connects the acetic acid
The residual air of the gas phase entrance of ethyl ester rectifying column first-stage condenser, the ethyl acetate rectifying column first-stage condenser exports described in connection
The gas phase entrance of ethyl acetate rectifying column secondary condenser；The ethyl acetate rectifying column first-stage condenser and the ethyl acetate
The ethyl acetate gas of entrapped moisture is condensed into liquid and converged again from the outflow of respective cold liquid outlet by rectifying column secondary condenser
The entrance of the ethyl acetate rectifying column cooler is connected after stream, described in the outlet connection of the ethyl acetate rectifying column cooler
Import in the middle part of ethyl acetate rectifying column water distributing can is to send the ethyl acetate liquid of entrapped moisture into the ethyl acetate rectifying
Tower water distributing can is simultaneously separated into ethyl acetate layer and the methanol liquid layer containing moisture up and down；
Ethyl acetate rectifying column described in the logical acquisition piping connection of the light phase export of the ethyl acetate rectifying column water distributing can
For refluxing opening with the lower layer's ethyl acetate backflow that will separate into the ethyl acetate rectifying column, heavy out passes through foldback pipeline
The liquid mouth that returns for connecting the extraction heavy phase tank is conveyed to the extraction heavy phase with the methanol liquid that moisture is contained in isolated lower layer
Tank；The first extraction mouth of discharge ethyl acetate, the first extraction mouth connection are equipped in the bottom side of the ethyl acetate rectifying column
The entrance of the ethyl acetate finished product cooler, it is to be checked that the outlet of the ethyl acetate finished product cooler connects the ethyl acetate
Tank is will obtain finished product after isolated ethyl acetate cooling and be sent into ethyl acetate tank to be checked.
Beneficial effect using above-mentioned further scheme is: ethyl acetate extracted recycles out purity through rectification
99% or more ethyl acetate finished product.
Further, the first pneumatic control valve and the first dehydration are equipped on the acquisition pipeline and the foldback pipeline
Flowmeter.
Further, the reextraction device includes extracting rectifying tower reactor, extractive distillation column, the condensation of extractive distillation column level-one
Device, extractive distillation column secondary condenser and extracting rectifying tower reactor cooler；The outlet of the extraction heavy phase tank is pumped by heavy phase
Second mixture is conveyed to the extractive distillation column, the extractive distillation column by the feed inlet for connecting the extractive distillation column
It is equipped with and is passed through extraction water and enters agent mouth with extract the methanol in second mixture；It is equipped in the extracting rectifying tower reactor
It is passed through the steam inlet of steam, gaseous phase outlet connects the gas phase entrance of the extractive distillation column to heat second mixture
The ethyl acetate gas of entrapped moisture is isolated from the second mixture, and described in the leakage fluid dram connection of the extractive distillation column
The liquid return hole of extracting rectifying tower reactor after the ethyl acetate gas for isolating entrapped moisture from second mixture will extract
The methanol liquid containing moisture taken is conveyed to the extracting rectifying tower reactor；Discharge is equipped in the bottom side of the extracting rectifying tower reactor
Second extraction mouth of the methanol liquid containing moisture, the second extraction mouth connect entering for the extracting rectifying tower reactor cooler
Mouthful, the outlet of the extracting rectifying tower reactor cooler will be separated cold by the extracting rectifying tower reactor pump connection methanol rectifying system
But the methanol liquid containing moisture after is sent into the methanol rectifying system；
The gaseous phase outlet of the extractive distillation column connects the gas phase entrance of the extractive distillation column first-stage condenser, the extraction
The residual air of rectifying column first-stage condenser is taken to export the gas phase entrance for connecting the extractive distillation column secondary condenser；The extraction essence
It evaporates tower first-stage condenser and the extractive distillation column secondary condenser and the ethyl acetate gas of entrapped moisture is condensed into liquid simultaneously
It is flowed out from respective cold liquid outlet and is separated into two-way branch after converging, wherein branch described in the first via passes through return line and connects
To the extracting rectifying top of tower refluxing opening so that a part of entrapped moisture ethyl acetate redistillation, branch described in the second tunnel is logical
It crosses circulation line and connects the entrance of the extraction batch can so that the ethyl acetate liquid of another part entrapped moisture is sent into the extraction
Feeding tank mixing mother liquor.
Beneficial effect using above-mentioned further scheme is: aqueous phase dissolved extracted has most methanol and a small amount of
Ethyl acetate, then using water as extractant reextraction methanol therein, it is allowed to be separated into methanol liquid and ethyl acetate for subsequent
Rectifying separation.
Further, branch described in the second tunnel connects the entrance of ethyl acetate interphase tank by the circulation line, described
The entrance that the outlet of ethyl acetate interphase tank passes through the interphase pump connection extraction batch can.
Beneficial effect using above-mentioned further scheme is: the ethyl acetate mixing mother liquor of reextraction separation is divided again
From raising separative efficiency.
Further, the second pneumatic control valve and the second dehydration are equipped on the return line and the circulation line
Flowmeter.
Further, the methanol rectifying system includes methanol rectification tower reactor, methanol rectifying tower, the condensation of methanol rectifying tower level-one
Device, methanol rectifying tower secondary condenser, methanol rectifying tower cooler and methanol rectifying tower tank to be checked；The extracting rectifying tower reactor is cold
But the outlet of device connects the feed inlet in the middle part of the methanol rectifying tower by extracting rectifying tower reactor pump will contain moisture
Methanol liquid is sent into the methanol rectifying tower, and the steam inlet for being passed through steam, gas phase are equipped in the methanol rectification tower reactor
Outlet connects the gas phase entrance of the methanol rectifying tower to heat the methanol liquid containing moisture and isolate methanol gas, and
The leakage fluid dram of the methanol rectifying tower connects the liquid return hole of the methanol rectification tower reactor will remain after isolating methanol gas
Extraction raffinate be conveyed to the methanol rectification tower reactor and distill again；
The gaseous phase outlet of the methanol rectifying tower connects the gas phase entrance of the methanol rectifying tower first-stage condenser, the first
The residual air outlet of alcohol rectifying column first-stage condenser connects the gas phase entrance of the methanol rectifying tower secondary condenser；The methanol essence
It evaporates tower first-stage condenser and the methanol rectifying tower first-stage condenser and methanol gas is condensed into liquid from respective cold liquid outlet
The entrance of the methanol rectifying tower cooler is flowed out and connects after converging, the outlet of the methanol rectifying tower cooler connects institute's first
Alcohol rectifying column tank to be checked will obtain finished product after isolated methanol cooling and be sent into methanol rectifying tower tank to be checked.
Beneficial effect using above-mentioned further scheme is: it is isolated that the methanol liquid of reextraction separation carries out rectifying
The satisfactory cold finished product of methanol.
Detailed description of the invention
Fig. 1 is that overall structure of the invention is illustrated.
In attached drawing, parts list represented by the reference numerals are as follows:
1. ethyl acetate interphase tank, 2. interphases pump, 3. extraction batch cans, 4, extraction material pump, 5. extractant tanks, 6. extractions
Agent pump, 7, extraction light phase tank, 8. light phases pump, 9. extraction heavy phase tanks, 10. heavy phases pump, 11. three-level extractors, 12 primary pumps, 13.
Two stage pump, 14. triplexes, 15. ethyl acetate rectifying tower reactors, 16. ethyl acetate rectifying columns, 17. ethyl acetate rectifying column level-ones
Condenser, 18. ethyl acetate rectifying column secondary condensers, 19. ethyl acetate rectifying column coolers, 20. ethyl acetate rectifying columns
Water distributing can, 21. ethyl ethyl ester finished product coolers, 22. ethyl ethyl esters tank to be checked, 23. extracting rectifying tower reactors, 24. extractions
Take rectifying column, 25. extractive distillation column first-stage condensers, 26. extractive distillation column secondary condensers, 27. extracting rectifying tower reactors cooling
Device, 28, extracting rectifying tower reactor pump, 29. methanol rectification tower reactors, 30. methanol rectifying towers, 31. methanol rectifying tower first-stage condensers,
32. methanol rectifying tower secondary condenser, 33. methanol rectifying tower coolers, 34. methanol rectifying towers tank to be checked.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
As shown in Figure 1, a kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor, including one
Secondary extraction equipment, ethyl acetate rectification device, reextraction device and methanol rectifying system.On the single extraction device
Equipped with the liquid inlet for being passed through mother liquor, and the single extraction device is mixed with obtaining first after adding water multitple extraction to separate in mother liquor
Object and the second mixture are closed, first mixture contains small part water in mother liquor, most of ethyl acetate and small part methanol,
Contain water most of in mother liquor, small part ethyl acetate and most of methanol in second mixture.The single extraction dress
The different discharge ports set are separately connected the entrance of the ethyl acetate rectification device and the reextraction device, and then will
First mixture is conveyed to after the ethyl acetate rectification device passes through rectification and obtains ethyl acetate, will be described
Second mixture is conveyed to the reextraction device by obtaining the methanol liquid containing moisture after adding water extraction and separation.It is described
The outlet of reextraction device connects the entrance of the methanol rectifying system with by the isolated methanol liquid containing moisture
The methanol rectifying system is conveyed to by obtaining methanol after rectifying.
The single extraction device includes extraction batch can 3, extractant tank 5, extraction light phase tank 7, extraction heavy phase tank 9 and three-level
Extractor 11.The extraction batch can 3 is equipped with the liquid inlet, and outlet passes through the 4 connection three-level extractor of extraction material pump
11 level-one feed inlet.Extraction water is equipped in the extractant tank 5, outlet is extracted by the 6 connection three-level of extractant pump
The three-level feed inlet of device 11 is mixed with providing the extraction water of multitple extraction mother liquor to the three-level extractor 11 and obtaining described first
Close object and second mixture.The three-level light phase discharge port and level-one heavy phase discharge port of the three-level extractor 11 are separately connected
The entrance of the extraction light phase tank 7 and the extraction heavy phase tank 9, and then first mixture and second mixture are divided
It is not conveyed to the extraction light phase tank 7 and the extraction heavy phase tank 9.
The ethyl acetate rectification device includes ethyl acetate rectifying tower reactor 15, ethyl acetate rectifying column 16, acetic acid
Ethyl ester rectifying column first-stage condenser 17, ethyl acetate rectifying column secondary condenser 18, ethyl acetate rectifying column cooler 19, acetic acid
Ethyl ester rectifying column water distributing can 20, ethyl acetate finished product cooler 21 and ethyl acetate tank 22 to be checked.The extraction light phase tank 7 goes out
Mouth is by the feed inlet of the 8 connection ethyl acetate rectifying tower reactors 15 of light phase pump first mixture is conveyed to the second
Acetoacetic ester rectifying tower reactor 15, in the ethyl acetate rectifying tower reactor 15 be equipped be passed through steam with heat first mixture from
The steam inlet of the ethyl acetate gas of entrapped moisture is isolated in first mixture.The gas of the ethyl acetate rectifying tower reactor 15
Mutually it is described the ethyl acetate gas of entrapped moisture to be conveyed to connect the gas phase entrance of the ethyl acetate rectifying column 16 for outlet
Ethyl acetate rectifying column 16, liquid return hole connect the leakage fluid dram of the ethyl acetate rectifying column 16 to isolate entrapped moisture
Remaining extraction raffinate the ethyl acetate rectifying tower reactor 15 is conveyed to after ethyl acetate gas to distill again.The ethyl acetate essence
The gaseous phase outlet for evaporating tower 16 connects the gas phase entrance of the ethyl acetate rectifying column first-stage condenser 17, the ethyl acetate rectifying
The residual air outlet of tower first-stage condenser 17 connects the gas phase entrance of the ethyl acetate rectifying column secondary condenser 18.The acetic acid
Ethyl ester rectifying column first-stage condenser 17 and the ethyl acetate rectifying column secondary condenser 18 are by the ethyl acetate gas of entrapped moisture
Body is condensed into liquid and connects entering for the ethyl acetate rectifying column cooler 19 after converging again from the outflow of respective cold liquid outlet
Mouthful, the outlet of the ethyl acetate rectifying column cooler 19 connect the import at 20 middle part of the ethyl acetate rectifying column water distributing can with
The ethyl acetate liquid of entrapped moisture is sent into the ethyl acetate rectifying column water distributing can 20 and is separated into ethyl acetate layer up and down
With the methanol liquid layer containing moisture.Described in the logical acquisition piping connection of the light phase export of the ethyl acetate rectifying column water distributing can 20
The refluxing opening of ethyl acetate rectifying column 16 with the lower layer's ethyl acetate backflow that will separate into the ethyl acetate rectifying column 16,
The methanol solution for returning liquid mouth so that moisture is contained in isolated lower layer that heavy out passes through extraction heavy phase tank 9 described in foldback piping connection
Body is conveyed to the extraction heavy phase tank 9.Be equipped with discharge ethyl acetate in the bottom side of the ethyl acetate rectifying column 16 first is adopted
Outlet, the first extraction mouth connect the entrance of the ethyl acetate finished product cooler 21, the ethyl acetate finished product cooler
21 outlet connects the ethyl acetate tank 22 to be checked will obtain finished product after isolated ethyl acetate cooling and be sent into the second
Acetoacetic ester tank 22 to be checked.The first pneumatic control valve and the first dehydration are equipped on the acquisition pipeline and the foldback pipeline
Flowmeter.
The reextraction device includes extracting rectifying tower reactor 23, extractive distillation column 24, extractive distillation column first-stage condenser
25, extractive distillation column secondary condenser 26 and extracting rectifying tower reactor cooler 27.The outlet of the extraction heavy phase tank 9 passes through weight
Mutually second mixture is conveyed to the extractive distillation column 24 by the feed inlet of the 10 connection extractive distillation column 24 of pump, described
Extractive distillation column 24, which is equipped with, to be passed through extraction water and enters agent mouth with extract the methanol in second mixture.In the extraction essence
It evaporates tower reactor 23 and is equipped with the steam inlet for being passed through steam, gaseous phase outlet connects the gas phase entrance of the extractive distillation column 24 to add
Heat second mixture isolates the ethyl acetate gas of entrapped moisture, and the extractive distillation column from the second mixture
24 leakage fluid dram connects the liquid return hole of the extracting rectifying tower reactor 23 to incite somebody to action after the ethyl acetate gas for isolating entrapped moisture
The methanol liquid containing moisture extracted from second mixture is conveyed to the extracting rectifying tower reactor 23.In the extraction
The bottom side of rectifying tower reactor 23 is equipped with the second extraction mouth of methanol liquid of the discharge containing moisture, and described second produces described in mouth connection
The outlet of the entrance of extracting rectifying tower reactor cooler 27, the extracting rectifying tower reactor cooler 27 passes through extracting rectifying tower reactor pump 28
The methanol liquid feeding methanol rectifying system after cooling containing moisture will be separated by connecting the methanol rectifying system.It is described
The gaseous phase outlet of extractive distillation column 24 connects the gas phase entrance of the extractive distillation column first-stage condenser 25, the extractive distillation column
The residual air outlet of first-stage condenser 25 connects the gas phase entrance of the extractive distillation column secondary condenser 26.The extractive distillation column
The ethyl acetate gas of entrapped moisture is condensed into liquid simultaneously by first-stage condenser 25 and the extractive distillation column secondary condenser 26
It is flowed out from respective cold liquid outlet and is separated into two-way branch after converging, wherein branch described in the first via passes through return line and connects
To 24 top of the extractive distillation column refluxing opening so that a part of entrapped moisture ethyl acetate redistillation, branch described in the second tunnel
The entrance for extracting batch can 3 is connected by circulation line so that described in the ethyl acetate liquid feeding of another part entrapped moisture
It extracts batch can 3 and mixes mother liquor, specific as follows: branch described in the second tunnel connects ethyl acetate interphase tank by the circulation line
1 entrance, the entrance that the outlet of the ethyl acetate interphase tank 1 passes through 2 connection of the interphase pump extraction batch can 3.Institute
It states and is equipped with the second pneumatic control valve and the second dehydration flowmeter on return line and the circulation line.
The methanol rectifying system includes methanol rectification tower reactor 29, methanol rectifying tower 30, methanol rectifying tower first-stage condenser
31, methanol rectifying tower secondary condenser 32, methanol rectifying tower cooler 33 and methanol rectifying tower tank 34 to be checked.The extracting rectifying
The outlet of tower reactor cooler 27 by the feed inlet in the middle part of the 28 connection methanol rectifying tower 30 of extracting rectifying tower reactor pump with
Methanol liquid containing moisture is sent into the methanol rectifying tower 30, is equipped in the methanol rectification tower reactor 29 and is passed through steam
Steam inlet, gaseous phase outlet connect the gas phase entrance of the methanol rectifying tower 30 to heat the methanol liquid containing moisture and divide
Methanol gas is separated out, and the leakage fluid dram of the methanol rectifying tower 30 connects the liquid return hole of the methanol rectification tower reactor 29 to divide
It separates out and remaining extraction raffinate is conveyed to the methanol rectification tower reactor 29 after methanol gas distills again.The methanol rectifying tower 30
Gaseous phase outlet connects the gas phase entrance of the methanol rectifying tower first-stage condenser 31, the methanol rectifying tower first-stage condenser 31
Residual air outlet connects the gas phase entrance of the methanol rectifying tower secondary condenser 32.31 He of methanol rectifying tower first-stage condenser
Methanol gas is condensed into liquid and flows out from respective cold liquid outlet and connect after converging by the methanol rectifying tower first-stage condenser 31
The entrance of the methanol rectifying tower cooler 33 is connect, outlet connection institute's methanol rectifying tower of the methanol rectifying tower cooler 33 waits for
Inspection tank 34 will obtain finished product after isolated methanol cooling and be sent into methanol rectifying tower tank 34 to be checked.
One complete course of work of the device is described below:
First step mother liquor adds water to extract (single extraction device): by Cefotaxime Sodium produce in the mother liquor (moisture that generates
8%, ethyl acetate 83%, methanol 8.3%, other solid impurities 0.7%) extraction batch can 3 is squeezed into, extraction is added in extractant tank 5
Extractant pump 6 is opened in technique agent, that is, extraction water, and extraction water enters three-level extractor 11.Three-level extractor 11 have from top to bottom according to
Secondary is level-one, second level and three-level for the container of extraction, and every level-one all has feed inlet, heavy out and light phase export, and
And the feed inlet of firsts and seconds, by primary pump connection 12, the feed inlet of second level and three-level is connected by two stage pump 13, three-level
It is connected with the feed inlet of level-one by triplex 14.Three-level heavy phase, which has, is pumped into two by two stage pump 13 for three-level heavy phase when liquid level
Grade, second level heavy phase, which has, is pumped into level-one by primary pump 12 for second level heavy phase when liquid level.While second level heavy phase is pumped into level-one, open
Extraction material pump 4, mother liquor and second level heavy phase is mixed through same pipeline into level-one, when level-one light phase has liquid level, by level-one
Light phase is mixed into second level through same pipeline simultaneously by two stage pump 13 and three-level heavy phase；When second level light phase has liquid level, by second level
Light phase is mixed into three-level through same pipeline simultaneously by triplex 14 and extractant water.Since ethyl acetate is slightly soluble in water (15
DEG C, 8.5g/100g), methanol is dissolved in water, and ethyl acetate specific gravity is smaller than water, therefore mother liquor passes through in three-level extractor 11
3 grades of process water extraction after obtain the first mixture and the second mixture, wherein the first mixture it is aqueous<4%, ethyl acetate>
95%, methanol < 1%, the second mixture aqueous about 80%, ethyl acetate about 5%, methanol about 15%.Due to the first mixture phase
Specific gravity compared with the second mixture is smaller, so the first mixture is discharged into extraction light phase tank 7 from three-level light phase discharge port, from the
Two mixture level-one heavy phase discharge ports, which are discharged into, is put into extraction heavy phase tank 9.By above-mentioned multitple extraction technique, substantially by mother liquor
In methanol extract in heavy phase water (the second mixture), realize methanol and ethyl acetate separation.Light phase acetic acid second in mother liquor
Ester (the first mixture) contains methanol < 1%, can recycle ethyl acetate through ethyl ester rectifying column 16.
The first mixture of second step rectification recycles ethyl acetate (ethyl acetate rectification device): extraction light phase tank
It is aqueous in 5<4%, ethyl acetate>95%, methanol<1% the first mixture ethyl acetate rectifying column 8 is fed to by light phase pump
Kettle 15 carries out batch fractionating: ethyl acetate rectifying tower reactor 15 has U-shaped heating tube bundle and collet, and the steam of 0.45-0.60Mpa is logical
Enter U-shaped heating tube bundle and collet heating extraction light phase feed liquid i.e. the first mixture, pneumatic control valve adjusts quantity of steam 400-
800kg/h.Because of ethyl acetate and methanol azeotropic and the low boiling point than water under normal circumstances, even if ethyl acetate rectifying
When temperature reaches the azeotropic point of ethyl acetate and methanol in tower reactor 15, due to the methanol in the first mixture be dissolved in water without
It can evaporate, ethyl acetate is heated in the first mixture becomes gas phase and sequentially enter ethyl acetate rectifying column first-stage condenser 17 and second
Acetoacetic ester rectifying column secondary condenser 18.17 collet of ethyl acetate rectifying column first-stage condenser leads to recirculated water, ethyl acetate rectifying
18 collet of tower secondary condenser leads to 7 DEG C of water and changes the ethyl acetate gas phase being thermally formed in ethyl acetate rectifying tower reactor 15
Heat condensation, recirculated water, 7 DEG C of water walk ethyl acetate rectifying column first-stage condenser 17 or ethyl acetate rectifying column secondary condenser 18
Tube layer, ethyl acetate gas phase walk the shell of ethyl acetate rectifying column first-stage condenser 17 and ethyl acetate rectifying column secondary condenser 18
Journey.It is cold that ethyl acetate gas phase walks ethyl acetate rectifying column first-stage condenser 17 and ethyl acetate rectifying column secondary condenser 18 exchanges heat
The acetic acid ethyl fluid that solidifying fraction is mingled with moisture communicates subcooling condensate and exports the shell into ethyl acetate rectifying column cooler 19,
The tube layer of ethyl acetate rectifying column cooler 19 is led to 7 DEG C of water and is cooled down to ethyl acetate fraction.It is cold through ethyl acetate rectifying column
But the ethyl acetate liquid phase after cooling for being mingled with moisture of device 19 divides water into ethyl acetate rectifying column water distributing can 20: passing through acetic acid second
Ester is less than the specific gravity of aqueous, and ethyl acetate is in the upper layer light phase of ethyl ester rectifying column water distributing can 20, and aqueous is in ethyl ester rectifying column
Lower layer's heavy phase of water distributing can 20.Upper layer light phase ethyl acetate flows back into ethyl ester rectifying column from 16 overhead reflux mouth of ethyl ester rectifying column
16, lower layer's heavy phase aqueous intermittent discharge is put into extraction heavy phase tank 9.After ethyl acetate rectifying column water distributing can 20 divides water, protect
Hold 77-85 DEG C, 0-15KPa of pressure of 15 temperature of ethyl ester rectifying tower reactor, in 77-82 DEG C of 16 column bottom temperature of ethyl ester rectifying column, tower under
It is 75.5-80 DEG C of temperature, cold through ethyl acetate finished product from the side line first of 16 tower bottom of ethyl ester rectifying column extraction mouth extraction ethyl acetate
But device 21 is discharged into ethyl acetate tank 22 to be checked after being cooled to finished product.
Third step extracts the second mixture separating acetic acid ethyl ester and methanol (reextraction device): in extraction heavy phase tank 9
Feed liquid i.e. the second mixture contains ethyl acetate about 5%, methanol about 15%, and water 80% separates its methanol using extracting rectifying mode
A small amount of ethyl acetate in water.Second mixture is fed to extractive distillation column 24 through heavy phase pump 10, and pneumatic control valve controls flow
1500-3000L/h, the U-shaped heating tube bundle and collet mouth of extracting rectifying tower reactor 23 lead to the heating of 0.45-0.60Mpa steam, pneumatically
Adjust 500-1000kg/h of valve regulation quantity of steam.25 tube layer of extractive distillation column first-stage condenser leads to recirculated water, extractive distillation column two
The tube layer of grade condenser 26 leads to 7 degree of water and carries out heat exchange condensation to the gas phase of shell.Extractant water is from extractive distillation column 24
Technique waterpipe is entered agent mouth and enters extractive distillation column 24, by the in the extractive distillation column 24 under the action of extractant water
Methanol extraction in two mixtures simultaneously takes in extracting rectifying tower reactor 23, and valve controls the flow 750-of extractant water
1000L/h.Ethyl acetate in second mixture heats in extractive distillation column 24 becomes gas phase.When 24 tower top of extractive distillation column
When 68-71 DEG C, 0-5Kpa of pressure, extractive distillation column first-stage condenser 25 and extractive distillation column secondary condenser 26 are mixed second
The ethyl acetate vapor condensation isolated of object is closed into ethyl acetate liquid, then again from respective condensate outlet by ethyl acetate
Liquid is sent into ethyl acetate interphase tank 1, and then produces the ethyl acetate interphase containing 1% or so methanol into ethyl acetate
Between phase tank 1, pneumatic control valve control extraction flow 800L/h.The interphase produced in ethyl acetate interphase tank 1 is in
Between mutually pump 2 be pumped into extraction batch can 3 be mixed into mother liquor carry out multitple extraction.When 23 temperature of extracting rectifying tower reactor reaches 83 DEG C or more, pressure
When 0-15Kpa of power, inside be then methanol and aqueous systems, methanol and aqueous systems squeeze into methanol by extracting rectifying tower reactor pump 28
Rectifying column 30.
Methanol first (methanol rectifying system) is recycled in 4th step rectifying: methanol rectification tower reactor 29 has U-shaped heating tube bundle and collet,
By U-shaped heating nozzle and collet mouth lead to the heating of 0.45-0.60Mpa steam be extracted 28 methanol squeezed into of rectifying tower reactor pump and
Aqueous systems, pneumatic control valve control 500-900kg/h of quantity of steam.Methanol in methanol and aqueous systems is heated and becomes methanol vapor phase
It is successively condensed again through methanol rectification tower top first-stage condenser 31 and methanol rectification tower top secondary condenser 32, water and other solids are miscellaneous
Matter (the 0.7% of mother liquor) rests in methanol rectification tower reactor 29 as discharge of wastewater to Sewage Disposal.Methanol rectification tower top one
Grade 31 tube layer of condenser leads to methanol vapor phase heat exchange condensation of the recirculated water to shell, and methanol rectifying tower secondary condenser 32 leads to 7 DEG C of water
It exchanges heat and condenses to the methanol vapor phase of shell.With the heating of steam, feed liquid, that is, extracting rectifying tower reactor pumps 28 in methanol rectifying tower 29
Squeeze into methanol and aqueous systems temperature rise, methanol rectification tower top first-stage condenser 31 and methanol rectification tower top secondary condenser
After 32 condensate liquid mouths have condensate liquid, condensate liquid flows back into methanol by the pipeline connecting with 29 overhead reflux mouth of methanol rectifying tower
Rectifying column 30.It flows back after 10-20min, when 63-64.5 DEG C of 30 tower top temperature of methanol rectifying tower, 0-5KPa of pressure, passes through
The pipeline connecting with methanol rectifying tower 34 feed inlet of tank to be checked produces qualified methanol, the pneumatic control valve control of extraction pipeline installation
Produce 200-500L/h of flow.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor, which is characterized in that including one
Secondary extraction equipment, ethyl acetate rectification device, reextraction device and methanol rectifying system；On the single extraction device
Equipped with the liquid inlet for being passed through mother liquor, and the single extraction device is mixed with obtaining first after adding water multitple extraction to separate in mother liquor
Object and the second mixture are closed, first mixture contains small part water in mother liquor, most of ethyl acetate and small part methanol,
Contain water most of in mother liquor, small part ethyl acetate and most of methanol in second mixture；The single extraction dress
The different discharge ports set are separately connected the entrance of the ethyl acetate rectification device and the reextraction device, and then will
First mixture is conveyed to after the ethyl acetate rectification device passes through rectification and obtains ethyl acetate, will be described
Second mixture is conveyed to the reextraction device by obtaining the methanol liquid containing moisture after adding water extraction and separation；It is described
The outlet of reextraction device connects the entrance of the methanol rectifying system with by the isolated methanol liquid containing moisture
The methanol rectifying system is conveyed to by obtaining methanol after rectifying.
2. the device according to claim 1 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, the single extraction device includes extraction batch can (3), extractant tank (5), extraction light phase tank (7), extraction heavy phase tank
(9) and three-level extractor (11)；The extraction batch can (3) is equipped with the liquid inlet, and outlet passes through extraction material pump (4) connection
The level-one feed inlet of the three-level extractor (11)；Extraction water is equipped in the extractant tank (5), outlet is pumped by extractant
(6) the three-level feed inlet of the three-level extractor (11) is connected to provide multitple extraction mother liquor to the three-level extractor (11)
Extraction water simultaneously obtains first mixture and second mixture；The three-level light phase discharge port of the three-level extractor (11)
The entrance of extraction light phase tank (7) and extraction heavy phase tank (9) is separately connected with level-one heavy phase discharge port, and then will be described
First mixture and second mixture are conveyed to the extraction light phase tank (7) and the extraction heavy phase tank (9) respectively.
3. the device according to claim 2 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
Be characterized in that, the ethyl acetate rectification device include ethyl acetate rectifying tower reactor (15), ethyl acetate rectifying column (16),
Ethyl acetate rectifying column first-stage condenser (17), ethyl acetate rectifying column secondary condenser (18), ethyl acetate rectifying tower cooler
Device (19), ethyl acetate rectifying column water distributing can (20), ethyl acetate finished product cooler (21) and ethyl acetate tank to be checked (22)；Institute
The outlet of extraction light phase tank (7) is stated by the feed inlet of light phase pump (8) connection ethyl acetate rectifying tower reactor (15) with by institute
It states the first mixture and is conveyed to the ethyl acetate rectifying tower reactor (15), be equipped on the ethyl acetate rectifying tower reactor (15) logical
Enter steam to heat the steam for the ethyl acetate gas that first mixture isolates entrapped moisture from the first mixture and enter
Mouthful；The gaseous phase outlet of the ethyl acetate rectifying tower reactor (15) connects the gas phase entrance of the ethyl acetate rectifying column (16) to incite somebody to action
The ethyl acetate gas of entrapped moisture is conveyed to the ethyl acetate rectifying column (16), and liquid return hole connects the ethyl acetate essence
The leakage fluid dram of tower (16) is evaporated so that remaining extraction raffinate is conveyed to the acetic acid after the ethyl acetate gas for isolating entrapped moisture
Ethyl ester rectifying tower reactor (15) is distilled again；The gaseous phase outlet of the ethyl acetate rectifying column (16) connects the ethyl acetate rectifying
The residual air of the gas phase entrance of tower first-stage condenser (17), the ethyl acetate rectifying column first-stage condenser (17) exports described in connection
The gas phase entrance of ethyl acetate rectifying column secondary condenser (18)；The ethyl acetate rectifying column first-stage condenser (17) and described
The ethyl acetate gas of entrapped moisture is condensed into liquid and from respective cold liquid by ethyl acetate rectifying column secondary condenser (18)
Outlet outflow connects the entrance of the ethyl acetate rectifying column cooler (19), the ethyl acetate rectifying tower cooler after converging again
The outlet of device (19) connects the import in the middle part of the ethyl acetate rectifying column water distributing can (20) with by the ethyl acetate of entrapped moisture
Liquid is sent into the ethyl acetate rectifying column water distributing can (20) and is separated into ethyl acetate layer and the methanol solution containing moisture up and down
Body layer；
Ethyl acetate rectifying column described in the logical acquisition piping connection of the light phase export of the ethyl acetate rectifying column water distributing can (20)
(16) for refluxing opening with the lower layer's ethyl acetate backflow that will separate into the ethyl acetate rectifying column (16), heavy out is logical
The liquid mouth that returns for crossing extraction heavy phase tank (9) described in foldback piping connection is conveyed to the methanol liquid that moisture is contained in isolated lower layer
The extraction heavy phase tank (9)；It is equipped with the first extraction mouth of discharge ethyl acetate in the bottom side of the ethyl acetate rectifying column (16),
The first extraction mouth connects the entrance of the ethyl acetate finished product cooler (21), the ethyl acetate finished product cooler (21)
Outlet connect the ethyl acetate tank to be checked (22) with ethyl acetate that will be isolated it is cooling after obtain finished product and be sent into the second
Acetoacetic ester tank to be checked (22).
4. the device according to claim 3 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, the first pneumatic control valve and the first dehydration flow is equipped on the acquisition pipeline and the foldback pipeline
Meter.
5. the device according to claim 2 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, the reextraction device includes that extracting rectifying tower reactor (23), extractive distillation column (24), extractive distillation column level-one are cold
Condenser (25), extractive distillation column secondary condenser (26) and extracting rectifying tower reactor cooler (27)；Extraction heavy phase tank (9)
Outlet by heavy phase pump (10) connect the feed inlet of the extractive distillation column (24) second mixture is conveyed to it is described
Extractive distillation column (24), the extractive distillation column (24) are equipped with and are passed through extraction water to extract the methanol in second mixture
Enter agent mouth；The steam inlet for being passed through steam is equipped on the extracting rectifying tower reactor (23), gaseous phase outlet connects the extraction
The gas phase entrance of rectifying column (24) is taken to heat the acetic acid that second mixture isolates entrapped moisture from the second mixture
Ethyl ester gas, and the leakage fluid dram of the extractive distillation column (24) connects the liquid return hole of the extracting rectifying tower reactor (23) to divide
The methanol liquid containing moisture extracted from second mixture is conveyed after separating out the ethyl acetate gas of entrapped moisture
To the extracting rectifying tower reactor (23)；Methanol liquid of the discharge containing moisture is equipped in the bottom side of the extracting rectifying tower reactor (23)
The second extraction mouth, the second extraction mouth connects the entrance of the extracting rectifying tower reactor cooler (27), the extracting rectifying
The outlet of tower reactor cooler (27) will be separated after cooling by extracting rectifying tower reactor pump (28) the connection methanol rectifying system
Methanol liquid containing moisture is sent into the methanol rectifying system；
The gaseous phase outlet of the extractive distillation column (24) connects the gas phase entrance of the extractive distillation column first-stage condenser (25), institute
The gas phase for stating the residual air outlet connection extractive distillation column secondary condenser (26) of extractive distillation column first-stage condenser (25) enters
Mouthful；The extractive distillation column first-stage condenser (25) and the extractive distillation column secondary condenser (26) are by the acetic acid of entrapped moisture
Ethyl ester gas is condensed into liquid and is separated into two-way branch after flowing out and converge from respective cold liquid outlet, wherein described in the first via
Branch is connected to the refluxing opening at the top of the extractive distillation column (24) so that a part of entrapped moisture acetic acid second by return line
Ester redistillation, branch described in the second tunnel connect the entrance of extraction batch can (3) so that another part is carried secretly by circulation line
The ethyl acetate liquid of moisture is sent into the extraction batch can (3) and mixes mother liquor.
6. the device according to claim 5 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, entrance of the branch described in the second tunnel by circulation line connection ethyl acetate interphase tank (1), the acetic acid
The outlet of ethyl ester interphase tank (1) connects the entrance of extraction batch can (3) by interphase pump (2).
7. the device according to claim 5 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, the second pneumatic control valve and the second dehydration flow is equipped on the return line and the circulation line
Meter.
8. the device according to claim 5 that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor,
It is characterized in that, the methanol rectifying system includes that methanol rectification tower reactor (29), methanol rectifying tower (30), methanol rectifying tower level-one are cold
Condenser (31), methanol rectifying tower secondary condenser (32), methanol rectifying tower cooler (33) and methanol rectifying tower tank to be checked (34)；
The outlet of the extracting rectifying tower reactor cooler (27) pumps (28) by the extracting rectifying tower reactor and connects the methanol rectifying tower
(30) feed inlet in the middle part of will be will be sent into the methanol rectifying tower (30) containing the methanol liquid of moisture, in the methanol rectifying tower
Kettle (29) is equipped with the steam inlet for being passed through steam, and gaseous phase outlet connects the gas phase entrance of the methanol rectifying tower (30) to add
Methanol liquid of the heat containing moisture simultaneously isolates methanol gas, and the leakage fluid dram of the methanol rectifying tower (30) connects the first
The liquid return hole of alcohol rectifying tower reactor (29) is to be conveyed to the methanol rectification tower reactor for remaining extraction raffinate after isolating methanol gas
(29) it distills again；
The gaseous phase outlet of the methanol rectifying tower (30) connects the gas phase entrance of the methanol rectifying tower first-stage condenser (31), institute
The gas phase for stating the residual air outlet connection methanol rectifying tower secondary condenser (32) of methanol rectifying tower first-stage condenser (31) enters
Mouthful；Methanol gas is condensed by the methanol rectifying tower first-stage condenser (31) and the methanol rectifying tower first-stage condenser (31)
Liquid flows out from respective cold liquid outlet and connects after converging the entrance of the methanol rectifying tower cooler (33), the methanol essence
Outlet connection institute's methanol rectifying tower tank to be checked (34) for evaporating tower cooler device (33) will obtain finished product after isolated methanol cooling and send
Enter methanol rectifying tower tank to be checked (34).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910141230.2A CN109678669B (en) | 2019-02-26 | 2019-02-26 | Device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor |
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| CN201910141230.2A CN109678669B (en) | 2019-02-26 | 2019-02-26 | Device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4473444A (en) * | 1981-02-09 | 1984-09-25 | National Distillers And Chemical Corporation | Extractive distillation of alcohol-ester mixtures |
| CN1269253A (en) * | 1999-04-07 | 2000-10-11 | 中国科学院大连化学物理研究所 | Methanol and ethyl acetate separating method |
| CN102746147A (en) * | 2012-07-09 | 2012-10-24 | 重庆大学 | Method for separating and recovering ethyl acetate and methanol |
| CN105272819A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Purification method of methanol containing ethyl acetate impurity |
| CN209669094U (en) * | 2019-02-26 | 2019-11-22 | 广西科伦制药有限公司 | A kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004063203A1 (en) * | 2003-01-10 | 2004-07-29 | Orchid Chemicals & Pharmaceuticals Ltd | Process for the preparation of cefotaxime sodium |
-
2019
- 2019-02-26 CN CN201910141230.2A patent/CN109678669B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4473444A (en) * | 1981-02-09 | 1984-09-25 | National Distillers And Chemical Corporation | Extractive distillation of alcohol-ester mixtures |
| CN1269253A (en) * | 1999-04-07 | 2000-10-11 | 中国科学院大连化学物理研究所 | Methanol and ethyl acetate separating method |
| CN102746147A (en) * | 2012-07-09 | 2012-10-24 | 重庆大学 | Method for separating and recovering ethyl acetate and methanol |
| CN105272819A (en) * | 2014-07-03 | 2016-01-27 | 中国石油化工股份有限公司 | Purification method of methanol containing ethyl acetate impurity |
| CN209669094U (en) * | 2019-02-26 | 2019-11-22 | 广西科伦制药有限公司 | A kind of device that Cefotaxime Sodium is produced to ethyl acetate and separating methanol in mother liquor |
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