CN109678669B - Device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor - Google Patents
Device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor Download PDFInfo
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- CN109678669B CN109678669B CN201910141230.2A CN201910141230A CN109678669B CN 109678669 B CN109678669 B CN 109678669B CN 201910141230 A CN201910141230 A CN 201910141230A CN 109678669 B CN109678669 B CN 109678669B
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 849
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 669
- 239000012452 mother liquor Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 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 15
- 229960002727 cefotaxime sodium Drugs 0.000 title claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 244
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 163
- 239000007788 liquid Substances 0.000 claims abstract description 115
- 239000000203 mixture Substances 0.000 claims abstract description 82
- 238000000895 extractive distillation Methods 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000007792 addition Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 120
- 239000000543 intermediate Substances 0.000 description 13
- 230000001105 regulatory effect Effects 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 125000004494 ethyl ester group Chemical group 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229930186147 Cephalosporin Natural products 0.000 description 2
- 229940124587 cephalosporin Drugs 0.000 description 2
- 150000001780 cephalosporins Chemical class 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000588923 Citrobacter Species 0.000 description 1
- 241000588921 Enterobacteriaceae Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000588748 Klebsiella Species 0.000 description 1
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 1
- 241000588770 Proteus mirabilis Species 0.000 description 1
- 241000588767 Proteus vulgaris Species 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 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
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002038 ethyl acetate fraction Substances 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000010413 mother solution Substances 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
- 239000002994 raw material Substances 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
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor, which comprises a primary extraction device, an ethyl acetate rectification water diversion device, a secondary extraction device and a methanol rectification device; the primary extraction device is provided with a liquid inlet which is used for introducing mother liquid to separate the mother liquid to obtain a first mixture and a second mixture; different discharge ports of the primary extraction device are respectively connected with inlets of the ethyl acetate rectifying water diversion device and the secondary extraction device, so that ethyl acetate is obtained after the first mixture is rectified and diverted, and methanol liquid containing water is obtained after the second mixture is fed with water, extracted and separated; and the outlet of the secondary extraction device is connected with the inlet of the methanol rectifying device so as to rectify the separated methanol liquid containing water to obtain methanol. The device can recycle ethyl acetate finished products with purity of more than 99 percent and qualified methanol finished products.
Description
Technical Field
The invention relates to the technical field of chemical product separation, in particular to a device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor.
Background
Ethyl acetate is also known as ethyl acetate. Pure ethyl acetate is colorless and transparent liquid with pungent smell, has low toxicity, sweet taste, is easy to volatilize, is sensitive to air, can absorb water, and is slowly hydrolyzed to be in an acidic reaction, is a fine chemical product with wide application, has excellent solubility, and is therefore commonly used for producing chemical intermediates, in particular to being used as a common crystallization solvent in the synthesis of cephalosporin medicines.
The saturated monohydric alcohol with the simplest structure of methanol (dr, CH3 OH) has wide application, and is a basic organic chemical raw material and high-quality fuel. The method is mainly applied to the fields of fine chemical engineering, plastics and the like, is used for manufacturing various organic products such as formaldehyde, acetic acid, chloromethane, methyl ammonia, dimethyl sulfide and the like, and is also one of important raw materials of pesticides and medicines.
The cefotaxime is third generation cephalosporin, has broad antibacterial spectrum, and has strong activity on Escherichia coli, proteus mirabilis leucocyte, gram negative bacteria such as enterobacteriaceae bacteria such as Klebsiella and Salmonella. It also has good effect on Proteus vulgaris and Citrobacter. The cefotaxime sodium is produced by using ethyl acetate and methanol in an aseptic process, and mother liquor components generated in the production process are complex, wherein the mother liquor components comprise 8% of water, 83% of ethyl acetate, 8.3% of methanol and 0.7% of other solid impurities. In order to reduce the production cost, the ethyl acetate and the methanol in the mother solution are required to be separated and recovered to reach the quality level of secondary use, and meanwhile, the pressure of a sewage treatment tank is reduced, so that the treated sewage is ensured to reach the national emission standard. Methanol and ethyl acetate are azeotroped, the azeotropic point is 53.9 ℃, 17.6% of methanol and 82.4% of ethyl acetate are azeotroped. In the current rectification mode, only ethyl acetate in mother liquor is generally recycled, and methanol is used as an intermediate phase of azeotropic composition.
Disclosure of Invention
In order to more efficiently recycle ethyl acetate and methanol, improve the utilization rate and ensure that the quality meets the production and use requirements, the invention aims to provide a device for separating ethyl acetate from methanol in a mother liquor of cefotaxime sodium production, which uses water as an extractant, extracts methanol from an ethyl acetate system to a water system by a multistage extraction method, and completely separates the ethyl acetate from the methanol in the mother liquor of cefotaxime sodium production by rectification and extraction rectification modes, wherein the quality of the recycled ethyl acetate is as follows: the water content is less than 0.3 percent, the chromaticity is less than (Pt-Co) 10 units of standard colorimetric solution, the turbidity is less than 0.5#, and the purity of ethyl acetate is more than or equal to 99.0 percent; the mass of the methanol reaches the following weight: the water content is less than 0.3%, the chromaticity is less than (Pt-Co) 10 units of standard colorimetric solution, the turbidity is less than 0.5#, and the purity of methanol is more than or equal to 99.0%.
The technical scheme for solving the technical problems is as follows: a device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor comprises a primary extraction device, an ethyl acetate rectification water diversion device, a secondary extraction device and a methanol rectification device; the primary extraction device is provided with a liquid inlet for introducing mother liquor, and the primary extraction device is used for adding water into the mother liquor to perform multistage extraction and separation to obtain a first mixture and a second mixture, wherein the first mixture contains a small part of water, a large part of ethyl acetate and a small part of methanol in the mother liquor, and the second mixture contains a large part of water, a small part of ethyl acetate and a large part of methanol in the mother liquor; different discharge ports of the primary extraction device are respectively connected with inlets of the ethyl acetate rectification water diversion device and the secondary extraction device, so that the first mixture is conveyed to the ethyl acetate rectification water diversion device to obtain ethyl acetate after rectification water diversion, and the second mixture is conveyed to the secondary extraction device to obtain methanol liquid containing water after water addition, extraction and separation; and the outlet of the secondary extraction device is connected with the inlet of the methanol rectifying device so as to convey the separated methanol liquid containing water to the methanol rectifying device to obtain methanol after rectification.
The beneficial effects of the invention are as follows: the method is characterized in that by utilizing the characteristic that ethyl acetate is slightly dissolved in water (15 ℃,8.5g/100 g), methanol is dissolved in water, and the specific weight of ethyl acetate is smaller than that of water, water is used as an extracting agent, methanol in mother liquor is extracted into water through multistage extraction, the primary separation of ethyl acetate and methanol is realized, and the ethyl acetate after extraction is distilled and separated into ethyl acetate finished products with purity of more than 99 percent; the water phase after extraction is dissolved with most of methanol and a small amount of ethyl acetate, and then water is used as an extractant to carry out extraction and rectification, and finally, a qualified methanol finished product is recovered.
Based on the technical scheme, the invention can also be improved as follows:
further, the primary extraction device comprises an extraction tank, an extractant tank, an extraction light phase tank, an extraction heavy phase tank and a three-stage extractor; the extraction tank is provided with the liquid inlet, and the outlet of the liquid inlet is connected with a first-stage feed inlet of the three-stage extractor through an extraction pump; the extraction agent tank is internally provided with extraction water, and an outlet of the extraction agent tank is connected with a three-stage feed inlet of the three-stage extractor through an extraction agent pump so as to provide extraction water of multi-stage extraction mother liquor for the three-stage extractor and obtain the first mixture and the second mixture; the three-stage light phase discharge port and the one-stage heavy phase discharge port of the three-stage extractor are respectively connected with the inlets of the extraction light phase tank and the extraction heavy phase tank, so that the first mixture and the second mixture are respectively conveyed to the extraction light phase tank and the extraction heavy phase tank.
The beneficial effects of adopting the further scheme are as follows: the water is used as an extractant and is subjected to multistage extraction, and methanol in the mother liquor is extracted into the water, so that the primary separation of ethyl acetate (first mixture) and methanol (second mixture) is realized.
Further, the ethyl acetate rectification water diversion device comprises an ethyl acetate rectification tower kettle, an ethyl acetate rectification tower primary condenser, an ethyl acetate rectification tower secondary condenser, an ethyl acetate rectification tower cooler, an ethyl acetate rectification tower water diversion tank, an ethyl acetate finished product cooler and an ethyl acetate to-be-detected tank; the outlet of the extraction light phase tank is connected with the feed inlet of the ethyl acetate rectifying tower kettle through a light phase pump so as to convey the first mixture to the ethyl acetate rectifying tower kettle, and the ethyl acetate rectifying tower kettle is provided with a steam inlet which is communicated with steam so as to heat the first mixture and separate ethyl acetate gas with water from the first mixture; the gas phase outlet of the ethyl acetate rectifying tower kettle is connected with the gas phase inlet of the ethyl acetate rectifying tower to convey the ethyl acetate gas with water to the ethyl acetate rectifying tower, and the liquid return port of the ethyl acetate rectifying tower kettle is connected with the liquid outlet of the ethyl acetate rectifying tower to convey residual liquid to the ethyl acetate rectifying tower kettle for re-distillation after the ethyl acetate gas with water is separated; the gas phase outlet of the ethyl acetate rectifying tower is connected with the gas phase inlet of the first-stage condenser of the ethyl acetate rectifying tower, and the residual gas outlet of the first-stage condenser of the ethyl acetate rectifying tower is connected with the gas phase inlet of the second-stage condenser of the ethyl acetate rectifying tower; the ethyl acetate rectifying tower primary condenser and the ethyl acetate rectifying tower secondary condenser condense ethyl acetate gas with water into liquid, flow out from respective cold liquid outlets and are connected with an inlet of the ethyl acetate rectifying tower cooler after converging, and an outlet of the ethyl acetate rectifying tower cooler is connected with an inlet in the middle of the ethyl acetate rectifying tower water diversion tank so as to send the ethyl acetate liquid with water into the ethyl acetate rectifying tower water diversion tank and separate the ethyl acetate liquid into an ethyl acetate layer and a methanol liquid layer containing water up and down;
the light phase outlet of the ethyl acetate rectifying tower water distributing tank is connected with a reflux port of the ethyl acetate rectifying tower through a collecting pipeline so as to reflux the separated lower ethyl acetate into the ethyl acetate rectifying tower, and the heavy phase outlet of the ethyl acetate rectifying tower is connected with a liquid return port of the extraction heavy phase tank through a return pipeline so as to convey the separated lower methanol liquid containing water to the extraction heavy phase tank; the bottom side of the ethyl acetate rectifying tower is provided with a first extraction outlet for discharging ethyl acetate, the first extraction outlet is connected with an inlet of an ethyl acetate finished product cooler, and an outlet of the ethyl acetate finished product cooler is connected with the ethyl acetate to-be-detected tank so as to cool separated ethyl acetate to obtain a finished product and send the finished product into the ethyl acetate to-be-detected tank.
The beneficial effects of adopting the further scheme are as follows: and rectifying the extracted ethyl acetate, and separating water to recover ethyl acetate finished product with purity of more than 99%.
Further, a first pneumatic adjusting valve and a first dehydration flowmeter are arranged on the collecting pipeline and the returning pipeline.
Further, the secondary extraction device comprises an extraction rectifying tower kettle, an extraction rectifying tower, a primary condenser of the extraction rectifying tower, a secondary condenser of the extraction rectifying tower and a cooler of the extraction rectifying tower kettle; the outlet of the extraction heavy phase tank is connected with the feed inlet of the extraction rectifying tower through a heavy phase pump to convey the second mixture to the extraction rectifying tower, and the extraction rectifying tower is provided with an inlet for introducing extraction water to extract methanol in the second mixture; a steam inlet for introducing steam is arranged on the extraction rectifying tower kettle, a gas phase outlet of the extraction rectifying tower kettle is connected with the gas phase inlet of the extraction rectifying tower to heat the second mixture to separate ethyl acetate gas with water from the second mixture, and a liquid outlet of the extraction rectifying tower is connected with a liquid return port of the extraction rectifying tower kettle to convey methanol liquid containing water extracted from the second mixture to the extraction rectifying tower kettle after separating the ethyl acetate gas with water; a second extraction outlet for discharging the methanol liquid containing the moisture is arranged at the bottom side of the extraction rectifying tower kettle, the second extraction outlet is connected with an inlet of the extraction rectifying tower kettle cooler, and an outlet of the extraction rectifying tower kettle cooler is connected with the methanol rectifying device through an extraction rectifying tower kettle pump to send the separated and cooled methanol liquid containing the moisture into the methanol rectifying device;
the gas phase outlet of the extraction rectifying tower is connected with the gas phase inlet of the first-stage condenser of the extraction rectifying tower, and the residual gas outlet of the first-stage condenser of the extraction rectifying tower is connected with the gas phase inlet of the second-stage condenser of the extraction rectifying tower; the first-stage condenser of the extractive distillation tower and the second-stage condenser of the extractive distillation tower condense ethyl acetate gas with water into liquid, flow out from respective cold liquid outlets and are converged and then are divided into two branches, wherein the first branch is connected to a reflux port at the top of the extractive distillation tower through a reflux pipeline so as to redistille part of ethyl acetate with water, and the second branch is connected with an inlet of the extraction tank through a circulation pipeline so as to send the other part of ethyl acetate liquid with water into the mixed mother liquor of the extraction tank.
The beneficial effects of adopting the further scheme are as follows: the water phase after extraction is dissolved with a large part of methanol and a small amount of ethyl acetate, and then water is used as an extractant to extract the methanol in the water phase for the second time, so that the methanol is separated into methanol liquid and ethyl acetate for subsequent rectification and separation.
Further, the second branch is connected with an inlet of an ethyl acetate intermediate phase tank through the circulating pipeline, and an outlet of the ethyl acetate intermediate phase tank is connected with an inlet of the extraction tank through an intermediate phase pump.
The beneficial effects of adopting the further scheme are as follows: and the ethyl acetate mixed mother liquor separated by secondary extraction is separated again, so that the separation efficiency is improved.
Further, a second pneumatic adjusting valve and a second dehydration flowmeter are arranged on the return pipeline and the circulating pipeline.
Further, the methanol rectifying device comprises a methanol rectifying tower kettle, a methanol rectifying tower, a first-stage condenser of the methanol rectifying tower, a second-stage condenser of the methanol rectifying tower, a cooler of the methanol rectifying tower and a tank to be detected of the methanol rectifying tower; the outlet of the extraction rectifying tower kettle cooler is connected with the feeding port in the middle of the methanol rectifying tower through the extraction rectifying tower kettle pump so as to send the methanol liquid containing moisture into the methanol rectifying tower, a steam inlet for introducing steam is arranged on the methanol rectifying tower kettle, the gas phase outlet of the extraction rectifying tower kettle is connected with the gas phase inlet of the methanol rectifying tower so as to heat the methanol liquid containing moisture and separate out methanol gas, and the liquid outlet of the methanol rectifying tower is connected with the liquid return port of the methanol rectifying tower kettle so as to convey residual liquid to the methanol rectifying tower kettle for re-distillation after separating out the methanol gas;
the gas phase outlet of the methanol rectifying tower is connected with the gas phase inlet of the first-stage condenser of the methanol rectifying tower, and the residual gas outlet of the first-stage condenser of the methanol rectifying tower is connected with the gas phase inlet of the second-stage condenser of the methanol rectifying tower; the first-stage condenser of the methanol rectifying tower and the first-stage condenser of the methanol rectifying tower condense methanol gas into liquid, the liquid flows out from respective cold liquid outlets and is converged and then is connected with an inlet of the cooler of the methanol rectifying tower, an outlet of the cooler of the methanol rectifying tower is connected with a tank to be detected of the methanol rectifying tower, the separated methanol is cooled and then a finished product is obtained, and the finished product is sent into the tank to be detected of the methanol rectifying tower.
The beneficial effects of adopting the further scheme are as follows: and rectifying and separating the methanol liquid separated by the secondary extraction to obtain a methanol cold finished product meeting the requirements.
Drawings
Fig. 1 is a schematic overall structure of the present invention.
In the drawings, the list of components represented by the various numbers is as follows:
1. ethyl acetate intermediate phase tank, 2, intermediate phase pump, 3, extraction tank, 4, extraction material pump, 5, extractant tank, 6, extractant pump, 7, extraction light phase tank, 8, light phase pump, 9, extraction heavy phase tank, 10, heavy phase pump, 11, three-stage extractor, 12, 13, two-stage pump, 14, three-stage pump, 15, ethyl acetate rectifying tower kettle, 16, ethyl acetate rectifying tower, 17, ethyl acetate rectifying tower first-stage condenser, 18, ethyl acetate rectifying tower second-stage condenser, 19, ethyl acetate rectifying tower cooler, 20, ethyl acetate rectifying tower water-separating tank, 21, ethyl acetate finished product cooler, 22, ethyl acetate rectifying tower kettle, 23, extraction rectifying tower kettle, 24, extraction rectifying tower first-stage condenser, 26, extraction rectifying tower second-stage condenser, 27, extraction rectifying tower condenser, 28, extraction rectifying tower pump, 29, methanol rectifying tower, 30, methanol rectifying tower, 31, rectifying tower second-stage condenser, 33, and 34.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
As shown in figure 1, the device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor comprises a primary extraction device, an ethyl acetate rectification water diversion device, a secondary extraction device and a methanol rectification device. The primary extraction device is provided with a liquid inlet for introducing mother liquor, and the primary extraction device is used for adding water into the mother liquor to perform multistage extraction and separation to obtain a first mixture and a second mixture, wherein the first mixture contains a small part of water, a large part of ethyl acetate and a small part of methanol in the mother liquor, and the second mixture contains a large part of water, a small part of ethyl acetate and a large part of methanol in the mother liquor. Different discharge ports of the primary extraction device are respectively connected with inlets of the ethyl acetate rectification water diversion device and the secondary extraction device, so that the first mixture is conveyed to the ethyl acetate rectification water diversion device to obtain ethyl acetate after rectification water diversion, and the second mixture is conveyed to the secondary extraction device to obtain methanol liquid containing water after water extraction and separation. And the outlet of the secondary extraction device is connected with the inlet of the methanol rectifying device so as to convey the separated methanol liquid containing water to the methanol rectifying device to obtain methanol after rectification.
The primary extraction device comprises an extraction material tank 3, an extractant tank 5, an extraction light phase tank 7, an extraction heavy phase tank 9 and a three-stage extractor 11. The extraction tank 3 is provided with the liquid inlet, and the outlet of the liquid inlet is connected with a primary feed inlet of the tertiary extractor 11 through the extraction pump 4. The extractant tank 5 is internally provided with extraction water, and the outlet of the extraction water is connected with a three-stage feed inlet of the three-stage extractor 11 through an extractant pump 6 so as to provide extraction water of the multi-stage extraction mother liquor for the three-stage extractor 11 and obtain the first mixture and the second mixture. The third-stage light phase discharge port and the first-stage heavy phase discharge port of the third-stage extractor 11 are respectively connected with the inlets of the extraction light phase tank 7 and the extraction heavy phase tank 9, so that the first mixture and the second mixture are respectively conveyed to the extraction light phase tank 7 and the extraction heavy phase tank 9.
The ethyl acetate rectification water diversion device comprises an ethyl acetate rectification tower kettle 15, an ethyl acetate rectification tower 16, an ethyl acetate rectification tower primary condenser 17, an ethyl acetate rectification tower secondary condenser 18, an ethyl acetate rectification tower cooler 19, an ethyl acetate rectification tower water diversion tank 20, an ethyl acetate finished product cooler 21 and an ethyl acetate to-be-detected tank 22. The outlet of the extraction light phase tank 7 is connected with the feed inlet of the ethyl acetate rectifying tower kettle 15 through a light phase pump 8 so as to convey the first mixture to the ethyl acetate rectifying tower kettle 15, and the ethyl acetate rectifying tower kettle 15 is provided with a steam inlet which is used for introducing steam to heat the first mixture and separate ethyl acetate gas with water from the first mixture. The gas phase outlet of the ethyl acetate rectifying tower kettle 15 is connected with the gas phase inlet of the ethyl acetate rectifying tower 16 to convey the ethyl acetate gas with water to the ethyl acetate rectifying tower 16, and the liquid return port of the ethyl acetate rectifying tower kettle 15 is connected with the liquid outlet of the ethyl acetate rectifying tower 16 to convey the residual liquid to the ethyl acetate rectifying tower kettle 15 for re-distillation after the ethyl acetate gas with water is separated. The gas phase outlet of the ethyl acetate rectifying tower 16 is connected with the gas phase inlet of the ethyl acetate rectifying tower primary condenser 17, and the residual gas outlet of the ethyl acetate rectifying tower primary condenser 17 is connected with the gas phase inlet of the ethyl acetate rectifying tower secondary condenser 18. The ethyl acetate rectifying tower primary condenser 17 and the ethyl acetate rectifying tower secondary condenser 18 condense ethyl acetate gas with water into liquid, the liquid flows out from respective cold liquid outlets and is converged and then is connected with an inlet of the ethyl acetate rectifying tower cooler 19, and an outlet of the ethyl acetate rectifying tower cooler 19 is connected with an inlet in the middle of the ethyl acetate rectifying tower water diversion tank 20 so as to send the ethyl acetate liquid with water into the ethyl acetate rectifying tower water diversion tank 20 and separate the ethyl acetate liquid into an ethyl acetate layer and a methanol liquid layer containing water up and down. The light phase outlet of the ethyl acetate rectifying tower water diversion tank 20 is connected with a reflux port of the ethyl acetate rectifying tower 16 through a collecting pipeline so as to reflux the separated lower ethyl acetate into the ethyl acetate rectifying tower 16, and the heavy phase outlet of the ethyl acetate rectifying tower is connected with a liquid return port of the extraction heavy phase tank 9 through a return pipeline so as to convey the separated lower methanol liquid containing water to the extraction heavy phase tank 9. A first extraction port for discharging ethyl acetate is arranged at the bottom side of the ethyl acetate rectifying tower 16, the first extraction port is connected with an inlet of the ethyl acetate finished product cooler 21, and an outlet of the ethyl acetate finished product cooler 21 is connected with the ethyl acetate to-be-detected tank 22 so as to cool separated ethyl acetate to obtain a finished product and send the finished product into the ethyl acetate to-be-detected tank 22. And the collecting pipeline and the return pipeline are respectively provided with a first pneumatic regulating valve and a first dehydration flowmeter.
The secondary extraction device comprises an extraction rectifying tower kettle 23, an extraction rectifying tower 24, an extraction rectifying tower primary condenser 25, an extraction rectifying tower secondary condenser 26 and an extraction rectifying tower kettle cooler 27. The outlet of the heavy extraction phase tank 9 is connected with the feed inlet of the extraction rectifying tower 24 through a heavy phase pump 10 to convey the second mixture to the extraction rectifying tower 24, and the extraction rectifying tower 24 is provided with an inlet for introducing extraction water to extract methanol in the second mixture. The extraction rectifying tower kettle 23 is provided with a steam inlet for introducing steam, a gas phase outlet of the steam inlet is connected with a gas phase inlet of the extraction rectifying tower 24 to heat the second mixture to separate ethyl acetate gas with water from the second mixture, and a liquid outlet of the extraction rectifying tower 24 is connected with a liquid return port of the extraction rectifying tower kettle 23 to convey methanol liquid with water extracted from the second mixture to the extraction rectifying tower kettle 23 after separating the ethyl acetate gas with water. The bottom side of the extraction rectifying tower kettle 23 is provided with a second extraction outlet for discharging the methanol liquid containing water, the second extraction outlet is connected with the inlet of the extraction rectifying tower kettle cooler 27, and the outlet of the extraction rectifying tower kettle cooler 27 is connected with the methanol rectifying device through an extraction rectifying tower kettle pump 28 to send the separated and cooled methanol liquid containing water into the methanol rectifying device. The gas phase outlet of the extractive distillation column 24 is connected with the gas phase inlet of the extractive distillation column primary condenser 25, and the residual gas outlet of the extractive distillation column primary condenser 25 is connected with the gas phase inlet of the extractive distillation column secondary condenser 26. The first condenser 25 of the extractive distillation column and the second condenser 26 of the extractive distillation column condense the ethyl acetate gas with water into liquid, and flow out from the cold liquid outlets of the extractive distillation column and flow together to divide the liquid into two branches, wherein the first branch is connected to a reflux port at the top of the extractive distillation column 24 through a reflux pipeline so as to redistille a part of ethyl acetate with water, and the second branch is connected to an inlet of the extraction tank 3 through a circulation pipeline so as to send the other part of ethyl acetate liquid with water into the mixed mother liquid of the extraction tank 3, and the specific steps are as follows: the second branch is connected with the inlet of the ethyl acetate intermediate phase tank 1 through the circulating pipeline, and the outlet of the ethyl acetate intermediate phase tank 1 is connected with the inlet of the extraction tank 3 through the intermediate phase pump 2. And the return pipeline and the circulating pipeline are both provided with a second pneumatic regulating valve and a second dehydration flowmeter.
The methanol rectifying device comprises a methanol rectifying tower kettle 29, a methanol rectifying tower 30, a methanol rectifying tower primary condenser 31, a methanol rectifying tower secondary condenser 32, a methanol rectifying tower cooler 33 and a methanol rectifying tower to-be-detected tank 34. The outlet of the extraction rectifying tower kettle cooler 27 is connected with the feeding port in the middle of the methanol rectifying tower 30 through the extraction rectifying tower kettle pump 28 so as to send the methanol liquid containing moisture into the methanol rectifying tower 30, the methanol rectifying tower kettle 29 is provided with a steam inlet for introducing steam, the gas phase outlet of the steam inlet is connected with the gas phase inlet of the methanol rectifying tower 30 so as to heat the methanol liquid containing moisture and separate out methanol gas, and the liquid outlet of the methanol rectifying tower 30 is connected with the liquid return port of the methanol rectifying tower kettle 29 so as to convey residual liquid to the methanol rectifying tower kettle 29 for distillation again after separating out the methanol gas. The gas phase outlet of the methanol rectifying tower 30 is connected with the gas phase inlet of the first condenser 31 of the methanol rectifying tower, and the residual gas outlet of the first condenser 31 of the methanol rectifying tower is connected with the gas phase inlet of the second condenser 32 of the methanol rectifying tower. The first-stage condenser 31 of the methanol rectifying tower and the first-stage condenser 31 of the methanol rectifying tower condense the methanol gas into liquid, the liquid flows out from respective cold liquid outlets and is converged and then is connected with an inlet of the cooler 33 of the methanol rectifying tower, an outlet of the cooler 33 of the methanol rectifying tower is connected with the tank 34 to be detected of the methanol rectifying tower, the separated methanol is cooled and then a finished product is obtained and is sent into the tank 34 to be detected of the methanol rectifying tower.
The following describes a complete operation of the device:
the first step of mother liquor adding water extraction (primary extraction device): mother liquor (water content 8%, ethyl acetate 83%, methanol 8.3% and other solid impurities 0.7%) generated in the production of cefotaxime sodium is pumped into an extraction tank 3, an extraction process agent, namely extraction water, is added into an extraction agent tank 5, an extraction agent pump 6 is started, and the extraction water enters a three-stage extractor 11. The three-stage extractor 11 is provided with a container for extracting a first stage, a second stage and a third stage from bottom to top, wherein each stage is provided with a feed inlet, a heavy phase outlet and a light phase outlet, the feed inlets of the first stage and the second stage are connected through a first-stage pump 12, the feed inlets of the second stage and the third stage are connected through a second-stage pump 13, and the feed inlets of the third stage and the first stage are connected through a third-stage pump 14. The tertiary heavy phase is pumped into the secondary stage by the secondary pump 13 when there is a liquid level in the tertiary heavy phase, and the secondary heavy phase is pumped into the primary stage by the primary pump 12 when there is a liquid level in the secondary heavy phase. The extraction and material taking pump 4 is started while the secondary heavy phase is pumped into the first stage, mother liquor and the secondary heavy phase are mixed together through the same pipeline to enter the first stage, and when the liquid level of the primary light phase exists, the primary light phase is mixed through the second stage pump 13 and the tertiary heavy phase through the same pipeline to enter the second stage; when the liquid level of the second light phase exists, the second light phase is mixed with extractant water through the three-stage pump 14 and the same pipeline at the same time to enter the three stages. Since ethyl acetate is slightly soluble in water (15 ℃,8.5g/100 g), methanol is soluble in water, and the specific gravity of ethyl acetate is less than that of water, the mother liquor is subjected to 3 stage extraction of process water in a three stage extractor 11 to obtain a first mixture and a second mixture, wherein the first mixture contains <4%, ethyl acetate >95%, methanol <1%, the second mixture contains about 80%, ethyl acetate about 5%, and methanol about 15%. Since the first mixture has a lower specific gravity than the second mixture, the first mixture is discharged from the third-stage light phase discharge port to the extraction light phase tank 7, and from the second mixture first-stage heavy phase discharge port to the put-in extraction heavy phase tank 9. By the multistage extraction process, the methanol in the mother liquor is basically extracted into heavy phase water (second mixture) to realize the separation of the methanol and the ethyl acetate. The light phase ethyl acetate (first mixture) in the mother liquor contains <1% methanol and ethyl acetate can be recovered via ethyl ester rectification column 16.
The second step of rectifying and water separating the first mixture to recover ethyl acetate (ethyl acetate rectifying and water separating device): the first mixture containing water <4%, ethyl acetate >95% and methanol <1% in the extraction light phase tank 5 is fed into an ethyl acetate rectifying tower kettle 15 through a light phase pump 8 for batch rectification: the ethyl acetate rectifying tower kettle 15 is provided with a U-shaped heating tube bundle and a jacket, 0.45-0.60 Mpa steam is introduced into the U-shaped heating tube bundle and the jacket to heat and extract light phase feed liquid, namely a first mixture, and a pneumatic regulating valve is used for regulating the steam quantity to 400-800 kg/h. Because ethyl acetate and methanol are azeotroped under normal conditions and have a boiling point lower than that of water, even when the temperature in the ethyl acetate rectifying column tank 15 reaches the azeotropic point of ethyl acetate and methanol, the ethyl acetate in the first mixture is changed into a gas phase by heat to enter the ethyl acetate rectifying column primary condenser 17 and the ethyl acetate rectifying column secondary condenser 18 in this order because the methanol in the first mixture is dissolved in water and does not evaporate. The jacket of the first condenser 17 of the ethyl acetate rectifying tower is filled with circulating water, the jacket of the second condenser 18 of the ethyl acetate rectifying tower is filled with water at 7 ℃ to exchange heat and condense ethyl acetate gas phase formed by heating in the ethyl acetate rectifying tower kettle 15, the circulating water and the water at 7 ℃ pass through the pipe layers of the first condenser 17 of the ethyl acetate rectifying tower or the second condenser 18 of the ethyl acetate rectifying tower, and the ethyl acetate gas phase passes through the shell passes of the first condenser 17 of the ethyl acetate rectifying tower and the second condenser 18 of the ethyl acetate rectifying tower. The ethyl acetate gas phase is taken away from the shell layer of the ethyl acetate rectifying tower cooler 19 through a condensate outlet, and the ethyl acetate fraction is cooled by water at 7 ℃ through the pipe layer of the ethyl acetate rectifying tower cooler 19. The ethyl acetate liquid phase mixed with water after being cooled by the ethyl acetate rectifying tower cooler 19 enters the ethyl acetate rectifying tower water diversion tank 20 for diversion: that is, the ethyl acetate is in the upper light phase of the ethyl ester rectifying tower water separating tank 20 and the water liquid is in the lower heavy phase of the ethyl ester rectifying tower water separating tank 20 by the specific gravity of the ethyl acetate being smaller than that of the water liquid. The upper light phase ethyl acetate flows back into the ethyl ester rectifying tower 16 from a reflux port at the top of the ethyl ester rectifying tower 16, and the lower heavy phase water is intermittently discharged and placed into the extraction heavy phase tank 9. After water is separated by the ethyl acetate rectifying tower water separating tank 20, the temperature of the ethyl acetate rectifying tower kettle 15 is kept at 77-85 ℃, the pressure is kept at 0-15 KPa, the temperature of the bottom of the ethyl acetate rectifying tower 16 is kept at 77-82 ℃, the middle lower temperature of the tower is kept at 75.5-80 ℃, ethyl acetate is extracted from a side line first extraction port at the bottom of the ethyl acetate rectifying tower 16, cooled into a finished product by an ethyl acetate finished product cooler 21, and then discharged into an ethyl acetate to-be-detected tank 22.
Third step extraction of the second mixture ethyl acetate and methanol (secondary extraction device): the feed solution in the heavy phase extraction tank 9, namely the second mixture, contains about 5% of ethyl acetate, about 15% of methanol and 80% of water, and a small amount of ethyl acetate in the methanol water is separated by adopting an extraction and rectification mode. The second mixture is fed into the extraction rectifying tower 24 through the heavy phase pump 10, the flow rate is controlled to be 1500-3000L/h by the pneumatic regulating valve, the U-shaped heating tube bundle and the jacket opening of the extraction rectifying tower kettle 23 are heated by 0.45-0.60 Mpa of steam, and the steam quantity is regulated to be 500-1000 kg/h by the pneumatic regulating valve. Circulating water is led into the pipe layer of the primary condenser 25 of the extraction rectifying tower, 7-DEG water is led into the pipe layer of the secondary condenser 26 of the extraction rectifying tower, and heat exchange condensation is carried out on the gas phase of the shell layer. The extractant water enters the extraction rectifying tower 24 from a process water pipeline in the extraction rectifying tower 24 through an inlet, the methanol in the second mixture in the extraction rectifying tower 24 is extracted and brought into the extraction rectifying tower kettle 23 under the action of the extractant water, and the flow rate of the extractant water is controlled to be 750-1000L/h by a valve. The ethyl acetate in the second mixture is heated to a vapor phase in extractive distillation column 24. When the temperature of the top 68-71 ℃ of the extraction rectifying tower 24 and the pressure of 0-5 Kpa are between 0 and 5Kpa, the ethyl acetate gas phase separated from the second mixture is condensed into ethyl acetate liquid by the first condenser 25 of the extraction rectifying tower and the second condenser 26 of the extraction rectifying tower, then the ethyl acetate liquid is sent into the ethyl acetate mesophase tank 1 from the respective condensate outlets, further the ethyl acetate mesophase containing about 1% of methanol is extracted into the ethyl acetate mesophase tank 1, and the extraction flow rate is controlled to be 800L/h by the pneumatic regulating valve. The intermediate phase extracted from the ethyl acetate intermediate phase tank 1 is pumped into an extraction tank 3 through an intermediate phase pump 2 and mixed with mother liquor for multistage extraction. When the temperature of the extraction rectifying tower kettle 23 reaches more than 83 ℃ and the pressure is 0-15 Kpa, a methanol and water system is arranged in the extraction rectifying tower kettle, and the methanol and water system is pumped into the methanol rectifying tower 30 through the extraction rectifying tower kettle pump 28.
And fourth step, rectifying and recovering methyl alcohol (methyl alcohol rectifying device): the methanol rectifying tower kettle 29 is provided with a U-shaped heating tube bundle and a jacket, 0.45-0.60 Mpa steam is introduced through the opening of the U-shaped heating tube and the opening of the jacket to heat a methanol and water system pumped by the extracting rectifying tower kettle pump 28, and the pneumatic regulating valve controls the steam quantity to be 500-900 kg/h. The methanol in the methanol and water system is subjected to heat change into a methanol gas phase, and then the methanol gas phase is condensed by a first condenser 31 at the top of the methanol rectifying tower and a second condenser 32 at the top of the methanol rectifying tower in sequence, and water and other solid impurities (0.7% of mother liquor) stay in a methanol rectifying tower kettle 29 to be discharged to a sewage treatment station as wastewater. The pipe layer of the first-stage condenser 31 at the top of the methanol rectifying tower is communicated with circulating water to perform heat exchange condensation on the methanol gas phase of the shell layer, and the second-stage condenser 32 at the top of the methanol rectifying tower is communicated with 7 ℃ water to perform heat exchange condensation on the methanol gas phase of the shell layer. With the heating of steam, the temperature of the feed liquid in the methanol rectifying tower 29, namely the temperature of the methanol and water system pumped in by the extraction rectifying tower kettle pump 28, rises, and after condensate is arranged at condensate ports of the first-stage condenser 31 and the second-stage condenser 32 at the top of the methanol rectifying tower, the condensate flows back into the methanol rectifying tower 30 through a pipeline connected with a reflux port at the top of the methanol rectifying tower 29. After 10-20 min of reflux, when the temperature at the top of the methanol rectifying tower 30 is 63-64.5 ℃ and the pressure is 0-5 KPa, qualified methanol is extracted through a pipeline connected with the feed inlet of the tank to be detected 34 of the methanol rectifying tower, and a pneumatic regulating valve arranged on the extraction pipeline controls the extraction flow to be 200-500L/h.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (4)
1. The device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor is characterized by comprising a primary extraction device, an ethyl acetate rectification water diversion device, a secondary extraction device and a methanol rectification device; the primary extraction device is provided with a liquid inlet for introducing mother liquor, and the primary extraction device is used for adding water into the mother liquor to perform multistage extraction and separation to obtain a first mixture and a second mixture, wherein the first mixture contains a small part of water, a large part of ethyl acetate and a small part of methanol in the mother liquor, and the second mixture contains a large part of water, a small part of ethyl acetate and a large part of methanol in the mother liquor; different discharge ports of the primary extraction device are respectively connected with inlets of the ethyl acetate rectification water diversion device and the secondary extraction device, so that the first mixture is conveyed to the ethyl acetate rectification water diversion device to obtain ethyl acetate after rectification water diversion, and the second mixture is conveyed to the secondary extraction device to obtain methanol liquid containing water after water addition, extraction and separation; the outlet of the secondary extraction device is connected with the inlet of the methanol rectifying device so as to convey the separated methanol liquid containing water to the methanol rectifying device to obtain methanol after rectification;
the primary extraction device comprises an extraction tank (3), an extractant tank (5), an extraction light phase tank (7), an extraction heavy phase tank (9) and a three-stage extractor (11); the extraction tank (3) is provided with the liquid inlet, and the outlet of the liquid inlet is connected with a first-stage feed inlet of the three-stage extractor (11) through an extraction pump (4); the extractant tank (5) is internally provided with extraction water, and an outlet of the extraction water is connected with a three-stage feed inlet of the three-stage extractor (11) through an extractant pump (6) so as to provide extraction water of the multi-stage extraction mother liquor for the three-stage extractor (11) and obtain the first mixture and the second mixture; the three-stage light phase discharge port and the one-stage heavy phase discharge port of the three-stage extractor (11) are respectively connected with the inlets of the extraction light phase tank (7) and the extraction heavy phase tank (9), so that the first mixture and the second mixture are respectively conveyed to the extraction light phase tank (7) and the extraction heavy phase tank (9);
the ethyl acetate rectification water diversion device comprises an ethyl acetate rectification tower kettle (15), an ethyl acetate rectification tower (16), an ethyl acetate rectification tower primary condenser (17), an ethyl acetate rectification tower secondary condenser (18), an ethyl acetate rectification tower cooler (19), an ethyl acetate rectification tower water diversion tank (20), an ethyl acetate finished product cooler (21) and an ethyl acetate to-be-detected tank (22); the outlet of the extraction light phase tank (7) is connected with the feed inlet of the ethyl acetate rectifying tower kettle (15) through a light phase pump (8) so as to convey the first mixture to the ethyl acetate rectifying tower kettle (15), and the ethyl acetate rectifying tower kettle (15) is provided with a steam inlet which is communicated with steam so as to heat the first mixture and separate ethyl acetate gas with water from the first mixture; the gas phase outlet of the ethyl acetate rectifying tower kettle (15) is connected with the gas phase inlet of the ethyl acetate rectifying tower (16) so as to convey the ethyl acetate gas with the water to the ethyl acetate rectifying tower (16), the liquid return port of the ethyl acetate rectifying tower kettle is connected with the liquid outlet of the ethyl acetate rectifying tower (16) so as to convey the residual liquid to the ethyl acetate rectifying tower kettle (15) for re-distillation after the ethyl acetate gas with the water is separated; the gas phase outlet of the ethyl acetate rectifying tower (16) is connected with the gas phase inlet of the first-stage condenser (17) of the ethyl acetate rectifying tower, and the residual gas outlet of the first-stage condenser (17) of the ethyl acetate rectifying tower is connected with the gas phase inlet of the second-stage condenser (18) of the ethyl acetate rectifying tower; the ethyl acetate rectifying tower primary condenser (17) and the ethyl acetate rectifying tower secondary condenser (18) condense ethyl acetate gas with water into liquid, flow out from respective cold liquid outlets and are connected with an inlet of the ethyl acetate rectifying tower cooler (19) after being converged, and an outlet of the ethyl acetate rectifying tower cooler (19) is connected with an inlet in the middle of the ethyl acetate rectifying tower water separating tank (20) so as to send the ethyl acetate liquid with water into the ethyl acetate rectifying tower water separating tank (20) and separate the ethyl acetate liquid into an ethyl acetate layer and a methanol liquid layer with water up and down;
the light phase outlet of the ethyl acetate rectifying tower water distributing tank (20) is connected with the reflux port of the ethyl acetate rectifying tower (16) through a collecting pipeline so as to reflux the separated lower ethyl acetate into the ethyl acetate rectifying tower (16), and the heavy phase outlet of the light phase outlet is connected with the liquid return port of the extraction heavy phase tank (9) through a return pipeline so as to convey the separated lower methanol liquid containing water to the extraction heavy phase tank (9); a first extraction outlet for discharging ethyl acetate is arranged at the bottom side of the ethyl acetate rectifying tower (16), the first extraction outlet is connected with an inlet of the ethyl acetate finished product cooler (21), and an outlet of the ethyl acetate finished product cooler (21) is connected with the ethyl acetate to-be-detected tank (22) so as to cool separated ethyl acetate to obtain a finished product and send the finished product into the ethyl acetate to-be-detected tank (22);
the secondary extraction device comprises an extraction rectifying tower kettle (23), an extraction rectifying tower (24), an extraction rectifying tower primary condenser (25), an extraction rectifying tower secondary condenser (26) and an extraction rectifying tower kettle cooler (27); the outlet of the extraction heavy phase tank (9) is connected with the feed inlet of the extraction rectifying tower (24) through a heavy phase pump (10) to convey the second mixture to the extraction rectifying tower (24), and the extraction rectifying tower (24) is provided with an inlet which is communicated with extraction water to extract methanol in the second mixture; a steam inlet for introducing steam is arranged on the extraction rectifying tower kettle (23), a gas phase outlet of the steam inlet is connected with a gas phase inlet of the extraction rectifying tower (24) so as to heat the second mixture to separate ethyl acetate gas with water from the second mixture, and a liquid outlet of the extraction rectifying tower (24) is connected with a liquid return port of the extraction rectifying tower kettle (23) so as to convey methanol liquid containing water extracted from the second mixture to the extraction rectifying tower kettle (23) after separating the ethyl acetate gas with water; a second extraction outlet for discharging the methanol liquid containing the moisture is arranged at the bottom side of the extraction rectifying tower kettle (23), the second extraction outlet is connected with an inlet of the extraction rectifying tower kettle cooler (27), and an outlet of the extraction rectifying tower kettle cooler (27) is connected with the methanol rectifying device through an extraction rectifying tower kettle pump (28) to send the separated and cooled methanol liquid containing the moisture into the methanol rectifying device;
the gas phase outlet of the extraction rectifying tower (24) is connected with the gas phase inlet of the extraction rectifying tower primary condenser (25), and the residual gas outlet of the extraction rectifying tower primary condenser (25) is connected with the gas phase inlet of the extraction rectifying tower secondary condenser (26); the first-stage condenser (25) of the extractive distillation tower and the second-stage condenser (26) of the extractive distillation tower condense ethyl acetate gas with water into liquid, flow out of respective cold liquid outlets and are converged and then are divided into two branches, wherein the first branch is connected to a reflux port at the top of the extractive distillation tower (24) through a reflux pipeline so as to redistille part of ethyl acetate with water, and the second branch is connected to an inlet of the extraction material tank (3) through a circulation pipeline so as to send the other part of ethyl acetate liquid with water into the mixed mother liquid of the extraction material tank (3);
the methanol rectifying device comprises a methanol rectifying tower kettle (29), a methanol rectifying tower (30), a methanol rectifying tower primary condenser (31), a methanol rectifying tower secondary condenser (32), a methanol rectifying tower cooler (33) and a methanol rectifying tower to-be-detected tank (34); the outlet of the extraction rectifying tower kettle cooler (27) is connected with the feeding port in the middle of the methanol rectifying tower (30) through the extraction rectifying tower kettle pump (28) so as to send methanol liquid containing moisture into the methanol rectifying tower (30), a steam inlet for introducing steam is arranged on the methanol rectifying tower kettle (29), the gas phase outlet of the extraction rectifying tower kettle cooler is connected with the gas phase inlet of the methanol rectifying tower (30) so as to heat the methanol liquid containing moisture and separate methanol gas, and the liquid outlet of the methanol rectifying tower (30) is connected with the liquid return port of the methanol rectifying tower kettle (29) so as to convey residual liquid to the methanol rectifying tower kettle (29) for re-distillation after separating the methanol gas;
the gas phase outlet of the methanol rectifying tower (30) is connected with the gas phase inlet of the first-stage condenser (31) of the methanol rectifying tower, and the residual gas outlet of the first-stage condenser (31) of the methanol rectifying tower is connected with the gas phase inlet of the second-stage condenser (32) of the methanol rectifying tower; the methanol rectifying tower primary condenser (31) and the methanol rectifying tower primary condenser (31) condense methanol gas into liquid, the liquid flows out from respective cold liquid outlets and is connected with an inlet of the methanol rectifying tower cooler (33) after converging, an outlet of the methanol rectifying tower cooler (33) is connected with a methanol rectifying tower to-be-detected tank (34) to cool separated methanol to obtain a finished product, and the finished product is sent into the methanol rectifying tower to-be-detected tank (34).
2. The device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor according to claim 1, wherein a first pneumatic adjusting valve and a first dehydration flowmeter are arranged on the collecting pipeline and the returning pipeline.
3. Device for separating ethyl acetate from methanol in a mother liquor for the production of cefotaxime sodium according to claim 1, characterized in that the second branch is connected to the inlet of an ethyl acetate intermediate phase tank (1) through the circulation line, and the outlet of the ethyl acetate intermediate phase tank (1) is connected to the inlet of the extraction tank (3) through an intermediate phase pump (2).
4. The device for separating ethyl acetate from methanol in cefotaxime sodium production mother liquor according to claim 1, wherein a second pneumatic adjusting valve and a second dehydration flowmeter are arranged on the return pipeline and the circulation pipeline.
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| 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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| US4473444A (en) * | 1981-02-09 | 1984-09-25 | National Distillers And Chemical Corporation | Extractive distillation of alcohol-ester mixtures |
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| WO2004063203A1 (en) * | 2003-01-10 | 2004-07-29 | Orchid Chemicals & Pharmaceuticals Ltd | Process for the preparation of cefotaxime sodium |
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