A clean recovery process for ceftriaxone acid mother liquor

Abstract

The present invention relates to the technical field of cefotaxime acid, and discloses a clean recovery process of cefotaxime acid mother liquor, wherein the mother liquor produced by preparing cefotaxime acid is filtered and treated by a nanofiltration membrane system to obtain a concentrated solution and a dialyzate; the concentrated solution is separated to obtain cefotaxime acid; the dialysate is pumped into the middle of a distillation tower through a raw material pump, and steam permeates to obtain high-purity ethanol. The pervaporation membrane device of the present invention dehydrates ethanol to a chemically pure level in one step, and has simple operation, high recovery rate and low energy consumption. After the clean recovery process, the purity of cefotaxime acid reaches more than 99.5%, and the purity of ethanol reaches more than 99.5%.

Description

Technical Field

[0001] The invention relates to the technical field of cefotaxime acid, in particular to a clean recovery process of cefotaxime acid mother liquor. Background Art

[0002] Ceftriaxone sodium is a third-generation semi-synthetic cephalosporin with an aminothiazolyl-cis-methoxyiminoacetyl group. Its antibacterial activity against Gram-negative bacteria and other bacteria is much stronger than that of first- and second-generation cephalosporins. It also has the advantages of low nephrotoxicity and relatively low price. It is currently a widely used antibiotic in clinical practice.

[0003] The industrial synthesis method of cefotaxime acid is the active ester method, with benzothiazole active ester as raw material, dichloromethane, tetrahydrofuran, etc. as solvent, under the action of a catalyst, condensation reaction with 7-aminocephalosporanic acid is carried out to obtain cefotaxime acid, and then reacted with sodium bicarbonate, sodium hydroxide, anhydrous sodium acetate, etc. to generate sodium salt, with a small amount of water as solvent, to generate water-soluble cefotaxime sodium, and then drop organic solvents such as anhydrous ethanol, acetone, isopropanol, etc., so that the crystals of cefotaxime sodium are fully precipitated to obtain the finished cefotaxime acid. There are processing defects in the above-mentioned route of synthesizing cefotaxime acid. Cefotaxime acid exists in the cefotaxime mother liquor, which will lead to a decrease in product yield. Excessive organic matter in the wastewater causes environmental pollution. If the traditional treatment method is used, it is almost impossible to effectively recover the economically valuable cefotaxime acid, and the organic solvent ethanol in the mother liquor cannot be economically and effectively recovered, which increases the economic and environmental burden of the enterprise. Summary of the invention

[0004] (I) Technical problems to be solved: The present invention provides a clean recovery process for cefotaxime acid mother liquor, which can economically, environmentally and effectively recover and reuse the active ingredient cefotaxime acid and organic solvent ethanol in the mother liquor of the cefotaxime acid synthesis process, and solves the problem of difficult treatment of cefotaxime acid mother liquor by simply combining nanofiltration membrane and permeation vapor membrane.

[0005] (II) Technical solution: A clean recovery process of cefotaxime acid mother liquor:

[0006] (1) The mother liquor produced by the preparation of cefotaxime acid is filtered through a plate and frame filter until the filtrate is clear and transparent without obvious solid impurities; the total mass concentration of the filtrate is controlled to be 0.3-0.8 mg / mL, the pH is 4-8, and the temperature is 15-30°C.

[0007] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the concentrate and dialysate are separated; the total mass concentration of the concentrate is controlled to be 10-25 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0008] (3) The concentrated liquid in the storage tank is purified in the production workshop, the pH is adjusted with hydrochloric acid, and the temperature is controlled to separate the cefotaxime acid; or the cefotaxime acid concentrated liquid is discharged into the material tank for application production.

[0009] (4) The dialysate is discharged into a distillation tower, and the ethanol in the dialysate is subjected to a pervaporation recovery process to obtain high-purity ethanol.

[0010] Furthermore, in (2), in the nanofiltration membrane treatment system, the filtration temperature is 15-35°C; the nanofiltration membrane nanofiltration purification operation pressure is 15-35 bar inlet pressure and 12-32 bar outlet pressure.

[0011] Furthermore, the molecular weight cutoff of the nanofiltration membrane is 400-600Da; diafiltration water is added to the cutoff side of the nanofiltration membrane, and the diafiltration multiple is 4-15 times that of the initial filtrate.

[0012] Furthermore, the nanofiltration membrane assembly is a roll membrane assembly or a tubular membrane assembly, and the nanofiltration membrane is a cross-linked wholly aromatic polyamide membrane.

[0013] Furthermore, in (3), the pH is adjusted to 3.5-6.5 with hydrochloric acid, and the temperature is controlled to 10-15°C.

[0014] Furthermore, in (4), the pervaporation recovery process is:

[0015] S1. The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60-70°C in a preheater, and then raised to 100-120°C to obtain a mixture of ethanol and water.

[0016] S2. The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 70-80%.

[0017] S3. Finally, the solution is passed through the steam permeation membrane assembly of the dehydration system for steam permeation, with the surface pressure of the interception side of the membrane being 0.5-0.8 MPa and the absolute pressure of the permeation side being 500-1500 Pa. The material on the interception side is condensed to obtain high-purity ethanol with a mass fraction greater than 99.5%.

[0018] Furthermore, the steam permeation membrane group is a rolled membrane assembly or a tubular membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane.

[0019] (III) Beneficial technical effects: Based on the clean recovery process of cefotaxime acid mother liquor, the present invention adds a mother liquor nanofiltration impurity removal process and a dialysate organic solvent permeation steam recovery process. The introduction of the above two process technologies realizes the economic, environmentally friendly and efficient recovery and utilization of cefotaxime acid, the active ingredient in the mother liquor of cefotaxime acid; and also realizes the economic, environmentally friendly and efficient recovery and utilization of ethanol, the organic solvent in the dialysate.

[0020] Compared with traditional processes, the nanofiltration concentration process can not only be carried out at low temperatures, thus avoiding the degradation reactions of chemical substances as much as possible, but also there is no phase change in the concentration process, and the concentration energy consumption is low. During the concentration, small molecular weight organic matter and inorganic salts such as sodium chloride can pass through the membrane, reducing the accumulation of impurities in the concentrate, and improving the purity and concentration of the reactant cefotaxime acid, which facilitates the next step of recovery and application.

[0021] The conventional process utilizes the azeotrope formed by ethanol-water in a distillation tower for dehydration, which has the disadvantages of low recovery rate, low purity, high energy consumption, etc. The dialysate treatment in the present invention uses a pervaporation membrane device to dehydrate ethanol to a chemically pure level in one step, which is simple to operate, has a high recovery rate, and low energy consumption. The cefotaxime acid mother liquor clean recovery process provided by the present invention is separated, and the purity of the cefotaxime acid is detected by HPLC high-performance liquid chromatography, and the purity of ethanol is detected by GC gas chromatography, and the purity can reach more than 99.54%. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] The nanofiltration membrane treatment system includes a material tank, a discharge valve, a raw material pump, a nanofiltration membrane treatment system, a pressure regulating valve, and a heat exchanger. After the filtrate passes through the process flow of the filtration membrane treatment system, a concentrated liquid and a dialysate are obtained.

[0024] The process flow of steam permeation membrane dehydration to ethanol includes a distillation tower, a reboiler, a superheater, a membrane assembly, a supplementary heat device, a condenser, a permeate, a permeate pump, a vacuum unit, a finished product cooler, a finished product, and a finished product pump. The dialysate is dehydrated through the process flow of steam permeation membrane dehydration to ethanol to obtain finished ethanol.

[0025] Example 1 Clean recovery process of cefotaxime acid mother liquor:

[0026] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.4 mg / mL, the pH to be 8, and the temperature to be 15°C.

[0027] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 15°C; the operating pressure of the nanofiltration membrane is 15 bar for inlet pressure and 12 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 400Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 4 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 25 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0028] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 5 with hydrochloric acid, and the temperature is controlled at 10°C to separate cefotaxime acid.

[0029] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 110°C to obtain a mixture of ethanol and water.

[0030] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 74%.

[0031] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 0.5 MPa, and the absolute pressure on the permeation side is 500 Pa. The material on the interception side is condensed to obtain high-purity ethanol.

[0032] Example 2 Clean recovery process of cefotaxime acid mother liquor:

[0033] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.3 mg / mL, the pH was 8, and the temperature was 30°C.

[0034] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 15°C; the operating pressure of the nanofiltration membrane is 35 bar for inlet pressure and 32 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 600Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 10 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 10 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0035] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 6.5 with hydrochloric acid, and the temperature is controlled at 15°C to separate cefotaxime acid.

[0036] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 120°C to obtain a mixture of ethanol and water.

[0037] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 80%.

[0038] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 0.8MPa, and the absolute pressure on the permeation side is 1500Pa. The material on the interception side is condensed to obtain high-purity ethanol.

[0039] Example 3 Clean recovery process of cefotaxime acid mother liquor:

[0040] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.3 mg / mL, the pH was 6, and the temperature was 15°C.

[0041] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 25°C; the operating pressure of the nanofiltration membrane is 22 bar for inlet pressure and 19 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 600Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 4 times that of the initial filtrate; the nanofiltration membrane component is a tubular membrane component, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 16 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0042] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 4 with hydrochloric acid, and the temperature is controlled at 15°C to separate cefotaxime acid.

[0043] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and is first heated to 65°C in a preheater and then to 100°C to obtain a mixture of ethanol and water.

[0044] (5) The ethanol and water mixture is sequentially passed through the series-connected membrane components of the distillation tower to obtain a solution with a mass fraction of 80%.

[0045] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a tubular membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 0.8 MPa, and the absolute pressure on the permeation side is 1500 Pa. The material on the interception side is condensed to obtain high-purity ethanol.

[0046] Example 4 Clean recovery process of cefotaxime acid mother liquor:

[0047] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.4 mg / mL, the pH was 6, and the temperature was 15°C.

[0048] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 25°C; the operating pressure of the nanofiltration membrane is 15 bar for inlet pressure and 12 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 600Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 10 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 18 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0049] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 3.5 with hydrochloric acid, and the temperature is controlled at 10°C to separate cefotaxime acid.

[0050] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and is first heated to 70°C in a preheater and then to 100°C to obtain a mixture of ethanol and water.

[0051] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 70%.

[0052] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 0.6MPa, and the absolute pressure on the permeation side is 1200Pa. The material on the interception side is condensed to obtain high-purity ethanol.

[0053] Example 5 Clean recovery process of cefotaxime acid mother liquor:

[0054] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.8 mg / mL, the pH was 4, and the temperature was 30°C.

[0055] (2) The filtrate is passed into the nanofiltration membrane treatment system to filter out impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 35°C; the operating pressure of the nanofiltration membrane purification is 22 bar for the inlet pressure and 19 bar for the outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 400Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 15 times that of the initial filtrate; the nanofiltration membrane component is a tubular membrane component, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 16 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0056] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 6.5 with hydrochloric acid, and the temperature is controlled at 15°C to separate cefotaxime acid.

[0057] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 110°C to obtain a mixture of ethanol and water.

[0058] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 77%.

[0059] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a tubular membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 0.5 MPa, and the absolute pressure on the permeation side is 500 Pa. The material on the interception side is condensed to obtain high-purity ethanol.

[0060] Comparative Example 1

[0061] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.2 mg / mL, the pH to be 8, and the temperature to be 15°C.

[0062] (2) The filtrate is passed into the nanofiltration membrane treatment system to filter out impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 15°C; the operating pressure of the nanofiltration membrane is 10 bar for inlet pressure and 7 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 400Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 4 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 6 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0063] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 2 with hydrochloric acid, and the temperature is controlled at 10°C to separate cefotaxime acid.

[0064] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 110°C to obtain a mixture of ethanol and water.

[0065] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 74%.

[0066] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the interception side of the membrane is 1MPa, and the absolute pressure on the permeation side is 1800Pa. The material on the interception side is condensed to obtain ethanol.

[0067] Comparative Example 2

[0068] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 1 mg / mL, the pH to be 8, and the temperature to be 15°C.

[0069] (2) The filtrate is passed into the nanofiltration membrane treatment system to filter out impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 15°C; the operating pressure of the nanofiltration membrane is 43 bar for inlet pressure and 40 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 400 Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 4 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 25 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0070] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 3 with hydrochloric acid, and the temperature is controlled at 25°C to separate cefotaxime acid.

[0071] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 110°C to obtain a mixture of ethanol and water.

[0072] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 74%.

[0073] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure of the retention side of the membrane is 0.5 MPa, and the absolute pressure of the permeation side is 500 Pa. The material on the retention side is condensed to obtain ethanol.

[0074] Comparative Example 3

[0075] (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities; the total mass concentration of the filtrate was controlled to be 0.2 mg / mL, the pH to be 8, and the temperature to be 40°C.

[0076] (2) The filtrate is passed into the nanofiltration membrane treatment system to remove impurities, calcium and magnesium ions, and the temperature during filtration is controlled at 15°C; the operating pressure of the nanofiltration membrane is 10 bar for inlet pressure and 7 bar for outlet pressure, and the molecular weight cutoff of the nanofiltration membrane is 400Da; diafiltration water is added to the interception side of the nanofiltration membrane, and the diafiltration multiple is 4 times that of the initial filtrate; the nanofiltration membrane assembly is a roll membrane assembly, and the nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialysate are separated; the total mass concentration of the concentrate is controlled to be 30 mg / mL. The concentrate is placed in a liquid storage tank and stored in a refrigerator.

[0077] (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 3 with hydrochloric acid, and the temperature is controlled at 10°C to separate cefotaxime acid.

[0078] (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 90°C to obtain a mixture of ethanol and water.

[0079] (5) The ethanol and water mixture is sequentially passed through the series membrane components of the distillation tower to obtain a solution with a mass fraction of 74%.

[0080] (6) The solution is steam permeated through the steam permeation membrane assembly of the dehydration system. The steam permeation membrane assembly is a roll-type membrane assembly, and the steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure of the interception side of the membrane is 0.4 MPa, and the absolute pressure of the permeation side is 400 Pa. The material on the interception side is condensed to obtain ethanol.

[0081] The purity of the cefotaxime acid obtained in step (3) is determined by HPLC high performance liquid chromatography, and the purity of the ethanol obtained in step (6) is determined by GC gas chromatography.

[0082] Table 1 Purity test of cefotaxime acid and ethanol

[0083]

[0084] As shown in Table 1, the purity of the cefotaxime acid separated in Examples 1 to 5 reached 99.51-99.78%, and the purity of ethanol reached 99.54-99.93%.

[0085] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A clean recovery process for cefotaxime acid mother liquor, characterized in that: The cleaning recovery process is: (1) The mother liquor produced by the preparation of cefotaxime acid was filtered through a plate and frame filter until the filtrate was clear and transparent without obvious solid impurities. The total mass concentration of the filtrate was controlled to be 0.8 mg / mL, the pH was 4, and the temperature was 30°C; (2) The filtrate is passed into the nanofiltration membrane treatment system to filter out impurities, calcium and magnesium ions. The temperature during filtration is controlled at 35°C. The operating pressure of the nanofiltration membrane purification is 22 bar for inlet pressure and 19 bar for outlet pressure. The molecular weight cutoff of the nanofiltration membrane is 400Da. Diafiltration water is added to the interception side of the nanofiltration membrane. The diafiltration multiple is 15 times that of the initial filtrate. The nanofiltration membrane assembly is a tubular membrane assembly. The nanofiltration membrane is a cross-linked fully aromatic polyamide membrane. The concentrate and the dialyzate are separated. The total mass concentration of the concentrate is controlled to be 16 mg / mL. The concentrate is placed in a liquid storage tank and stored in a cold storage room. (3) The concentrated liquid in the storage tank is placed in a purification production workshop, the pH value is adjusted to 6.5 with hydrochloric acid, and the temperature is controlled at 15°C to separate cefotaxime acid; (4) The dialysate is pumped into the middle of the distillation tower through a raw material pump, and the temperature is first raised to 60°C in a preheater and then raised to 110°C to obtain a mixture of ethanol and water; (5) Passing the mixture of ethanol and water through the series-connected membrane modules of the distillation tower in sequence to obtain a solution with a mass fraction of 77%; (6) The solution is passed through a steam permeation membrane assembly of a dehydration system for steam permeation. The steam permeation membrane assembly is a tubular membrane assembly. The steam permeation membrane is a water-permeable molecular sieve membrane. The surface pressure on the retention side of the membrane is 0.5 MPa, and the absolute pressure on the permeation side is 500 Pa. The material on the retention side is condensed to obtain ethanol.

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