Treatment method for recovering product from tazobactam crystallization mother liquor by membrane process

Abstract

The invention relates to the technical field of chemical processes, in particular to a treatment method for recovering products from tazobactam crystallization mother liquor by a membrane process, which comprises the following steps: S1, feeding the tazobactam crystallization mother liquor into an ultrafiltration ceramic membrane system, and removing solid particles from the tazobactam crystallization mother liquor by the ultrafiltration ceramic membrane system to obtain the tazobactam crystallization mother liquor; a pretreatment solution I and a high-solid-content ceramic membrane concentrated solution II are obtained; s2, the pretreatment liquid I is fed into a nanofiltration system for nanofiltration concentration, and nanofiltration concentrated liquid III and nanofiltration dialysate IV are obtained after the pretreatment liquid I is concentrated through the nanofiltration system; and S3, cooling the nano-filtration concentrated solution III in the S2, adding the nano-filtration concentrated solution III into the ceramic membrane concentrated solution II, standing, crystallizing, filtering and drying to obtain the product tazobactam and a secondary crystallization mother solution V. The method can effectively solve the problems that an existing treatment method is relatively high in energy consumption, relatively high in tazobactam production cost and relatively high in product purity due to the fact that relatively much tazobactam and water are easily wasted in the treatment process, and the like. And the production efficiency is low.

Description

Technical Field

[0001] The invention relates to the technical field of chemical process, in particular to a processing method for recovering products from tazobactam crystal mother liquor by using a membrane process. Background Art

[0002] Tazobactam, whose chemical name is: (2S,3S,5R)-3-methyl-7-oxo-3-(1H-1,2,3-triazol-1-ylmethyl)-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid. In the final step of the refining process of tazobactam, the product is recovered by cooling and crystallization to obtain the product tazobactam and tazobactam crystallization mother liquor; the crystallization mother liquor is distilled to recover ethanol, and tazobactam is converted into other substances (impurities) through high temperature and discharged to the sewage treatment plant together with water for treatment.

[0003] However, the existing treatment methods still have shortcomings, specifically: the existing treatment process consumes a lot of energy, and a lot of tazobactam and water are easily wasted in the treatment process, resulting in high production costs and low production efficiency of tazobactam.

[0004] Therefore, a method for recovering products from tazobactam crystallization mother liquor by a membrane process is needed to solve the problems raised in the above background technology. Summary of the invention

[0005] The object of the present invention is to provide a method for recovering products from tazobactam crystallization mother liquor by membrane process, so as to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solutions: A method for recovering a product from a tazobactam crystallization mother liquor by a membrane process comprises the following steps: S1, sending the tazobactam crystallization mother liquor into an ultrafiltration ceramic membrane system, the ultrafiltration ceramic membrane system removes solid particles from the tazobactam crystallization mother liquor to obtain a pretreated liquid I and a high-solid ceramic membrane concentrated liquid II; S2, sending the pre-treated liquid I into the nanofiltration system for nanofiltration concentration, and obtaining nanofiltration concentrated liquid III and nanofiltration dialyzate IV after concentration by the nanofiltration system; S3, cooling the nanofiltration concentrated solution III in S2, adding it to the ceramic membrane concentrated solution II, allowing it to stand, crystallize, filter and dry, to obtain the product tazobactam and the secondary crystallization mother solution V.

[0007] As a preferred solution of the present invention, the pore size of the ultrafiltration ceramic membrane in the ultrafiltration ceramic membrane system in S1 is 10 nm.

[0008] As a preferred solution of the present invention, the molecular weight of the nanofiltration membrane of the nanofiltration system in S2 is 100-500 Da1, the operating temperature of the nanofiltration system is 20-30°C, the pressure of the nanofiltration system is 0.5-3.0 MPa, and the concentration multiple of the nanofiltration system is 3-5 times.

[0009] As a preferred embodiment of the present invention, the content of tazobactam in the nanofiltration dialysate IV in S2 is less than 0.01%, and the nanofiltration dialysate IV is recycled for production, and more than 98% ethanol aqueous solution can be obtained in S2.

[0010] As a preferred solution of the present invention, the recovery rate of the product tazobactam in S3 is above 95%.

[0011] As a preferred embodiment of the present invention, the secondary crystallization mother liquor V in S3 can be further concentrated or returned to the next batch of tazobactam crystallization mother liquor to obtain the highest possible recovery rate of tazobactam.

[0012] As a preferred embodiment of the present invention, the secondary crystallization mother liquor V is subjected to a method of continuous concentration by subjecting the secondary crystallization mother liquor V to multiple crystallization treatments to obtain multiple crystallization mother liquors, and then the multiple crystallization mother liquors are distilled to obtain ethanol and hazardous waste, and the ethanol is recycled.

[0013] Compared with the prior art, the present invention has the following beneficial effects: 1. In the present invention, the tazobactam crystallization mother liquor is sent to an ultrafiltration ceramic membrane system, and the ultrafiltration ceramic membrane system removes solid particles from the tazobactam crystallization mother liquor to obtain a pretreatment liquid I and a high-solid ceramic membrane concentrated liquid II. The pretreatment liquid I is sent to a nanofiltration system for nanofiltration concentration, and after concentration by the nanofiltration system, a nanofiltration concentrated liquid III and a nanofiltration dialyzate IV are obtained. After the nanofiltration concentrated liquid III is cooled, it is added to the ceramic membrane concentrated liquid II for standing, crystallization, filtration and drying to obtain the product tazobactam and the secondary crystallization mother liquor V, and a physical method is used to achieve that small molecules such as water and ethanol pass through the nanofiltration membrane while tazobactam The macromolecules of tazobactam are intercepted, and the mother liquor of tazobactam crystallization is concentrated; the concentrated solution is added to the ceramic concentrated solution in the pretreatment, and then the concentrated solution is allowed to stand, filtered, and dried to recover part of the product tazobactam, and more than 90% of the product can be recovered; the concentrated dialysate ethanol aqueous solution can be returned to the upstream process section, which can avoid the energy consumption generated by distilling and recovering ethanol, not only realizing the recycling of solvents and reducing sewage treatment costs, but also recovering products to improve corporate benefits, solving the problems of high energy consumption in the existing treatment process, and easy waste of more tazobactam and water in the treatment process, resulting in high production cost and low production efficiency of tazobactam. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a schematic diagram of the process flow of the present invention. DETAILED DESCRIPTION

[0015] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0016] To facilitate understanding of the present invention, the present invention will be described more comprehensively below with reference to the relevant drawings, and several embodiments of the present invention are given. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

[0017] It should be noted that when an element is referred to as being "fixed on" another element, it may be directly on the other element or there may also be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used in this article are for illustrative purposes only.

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by technicians in the technical field to which the present invention belongs. The terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used in this article includes any and all combinations of one or more related listed items.

[0019] For examples, see Figure 1 , the present invention provides a technical solution: A method for recovering a product from a tazobactam crystallization mother liquor by a membrane process comprises the following steps: S1, sending the tazobactam crystallization mother liquor into an ultrafiltration ceramic membrane system, the ultrafiltration ceramic membrane system removes solid particles from the tazobactam crystallization mother liquor to obtain a pretreated liquid I and a high-solid ceramic membrane concentrated liquid II; S2, sending the pre-treated liquid I into the nanofiltration system for nanofiltration concentration, and obtaining nanofiltration concentrated liquid III and nanofiltration dialyzate IV after concentration by the nanofiltration system; S3, cooling the nanofiltration concentrated solution III in S2, adding it to the ceramic membrane concentrated solution II, allowing it to stand, crystallize, filter and dry, to obtain the product tazobactam and the secondary crystallization mother solution V.

[0020] Furthermore, the pore size of the ultrafiltration ceramic membrane in the ultrafiltration ceramic membrane system in S1 is 10 nm.

[0021] Furthermore, the molecular weight of the nanofiltration membrane of the nanofiltration system in S2 is 100-500 Da1, the operating temperature of the nanofiltration system is 20-30° C., the pressure of the nanofiltration system is 0.5-3.0 MPa, and the concentration multiple of the nanofiltration system is 3-5 times.

[0022] Furthermore, the content of tazobactam in the nanofiltration dialysate IV in S2 is less than 0.01%, and the nanofiltration dialysate IV is recycled for production, and more than 98% of ethanol aqueous solution can be obtained in S2.

[0023] Furthermore, the recovery rate of the product tazobactam in S3 is above 95%.

[0024] Furthermore, the secondary crystallization mother liquor V in S3 can be further concentrated or returned to the next batch of tazobactam crystallization mother liquor to obtain the highest possible recovery rate of tazobactam.

[0025] Furthermore, the secondary crystallization mother liquor V is subjected to a method of continuous concentration by subjecting the secondary crystallization mother liquor V to multiple crystallization treatments to obtain multiple crystallization mother liquors, and then the multiple crystallization mother liquors are distilled to obtain ethanol and hazardous waste, and the ethanol is recycled.

[0026] 100 kg of tazobactam crystallization mother liquor, wherein the content of tazobactam is 0.8%, is treated with a 10 m ultrafiltration ceramic membrane to obtain a pretreatment liquid I and a high-solid ceramic membrane concentrate II, the pretreatment liquid I is passed into a 500 Dal nanofiltration concentration system, and concentrated 5 times under environmental conditions of 0.5 MPa and 20-30 ° C to obtain a supersaturated concentrate III and a nanofiltration dialyzate VI, the supersaturated concentrate III is added to the high-solid ceramic membrane concentrate II, after cooling, the product tazobactam is allowed to stand, filtered, and dried to obtain a secondary crystallization mother liquor V, wherein the content of tazobactam in the nanofiltration dialyzate is 0.07%;

[0027] 100 kg of tazobactam crystallization mother liquor, wherein the content of tazobactam is 0.8%, is treated with a 10 m ultrafiltration ceramic membrane to obtain a pretreatment liquid I and a high-solid ceramic membrane concentrate II, the pretreatment liquid I is passed into a 100 Dal nanofiltration concentration system, and concentrated 3 times under environmental conditions of 3.0 MPa and 20-30 ° C to obtain a supersaturated concentrate III and a nanofiltration dialysate VI, the supersaturated concentrate III is added to the high-solid ceramic membrane concentrate II, after cooling, standing, filtering, and drying to obtain the product tazobactam and a secondary crystallization mother liquor V, wherein the content of tazobactam in the nanofiltration dialysate is 0;

[0028] 100 kg of tazobactam crystallization mother liquor, wherein the content of tazobactam is 0.8%, is treated with a 10 nm ultrafiltration ceramic membrane to obtain a pretreatment liquid I and a high solid content ceramic membrane concentrate II, the pretreatment liquid I is passed into a 200 Dal nanofiltration concentration system, and concentrated 5 times under environmental conditions of 2.0 MPa and 20-30 ° C to obtain a supersaturated concentrate III and a nanofiltration dialyzate VI, the supersaturated concentrate III is added to the high solid content ceramic membrane concentrate II, after cooling, standing, filtering, and drying to obtain the product tazobactam and a secondary crystallization mother liquor V, wherein the content of tazobactam in the nanofiltration dialysate is 0, and the obtained secondary crystallization mother liquor V is repeated with the process of Example 3, and after secondary concentration and crystallization, the recovery rate of tazobactam can reach 91.4%.

[0029] It can be seen from the specific implementation cases 1-3 that the present application scheme adopts a membrane process to concentrate the tazobactam crystallization mother liquor, and the process is a physical process with simple process, convenient operation and low energy consumption. The content of tazobactam in the nanofiltration dialysate is less than 0.01%, which reduces the steam consumption by 90%, greatly reduces the mother liquor treatment cost, and can recover more than 90% of the product tazobactam, thereby improving the enterprise efficiency. Moreover, the NF membrane core used can be completely regenerated after chemical cleaning and can be recycled.

[0030] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for recovering products from tazobactam crystallization mother liquor by membrane process, characterized in that: The following steps are involved: S1, sending the tazobactam crystallization mother liquor into an ultrafiltration ceramic membrane system, the ultrafiltration ceramic membrane system removes solid particles from the tazobactam crystallization mother liquor to obtain a pretreated liquid I and a high-solid ceramic membrane concentrated liquid II; S2, sending the pre-treated liquid I into the nanofiltration system for nanofiltration concentration, and obtaining nanofiltration concentrated liquid III and nanofiltration dialyzate IV after concentration by the nanofiltration system; S3, cooling the nanofiltration concentrated solution III in S2, adding it to the ceramic membrane concentrated solution II, allowing it to stand, crystallize, filter and dry, to obtain the product tazobactam and the secondary crystallization mother solution V.

2. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 1, characterized in that: The pore size of the ultrafiltration ceramic membrane in the ultrafiltration ceramic membrane system in S1 is 10 nm.

3. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 1, characterized in that: The molecular weight of the nanofiltration membrane of the nanofiltration system in S2 is 100-500 Da1, the operating temperature of the nanofiltration system is 20-30° C., the pressure of the nanofiltration system is 0.5-3.0 MPa, and the concentration multiple of the nanofiltration system is 3-5 times.

4. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 1, characterized in that: The content of tazobactam in the nanofiltration dialysate IV in S2 is less than 0.01%, and the nanofiltration dialysate IV is recycled for production, and more than 98% ethanol aqueous solution can be obtained in S2.

5. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 1, characterized in that: The recovery rate of the product tazobactam in S3 is above 95%.

6. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 1, characterized in that: The secondary crystallization mother liquor V in S3 can be further concentrated or returned to the next batch of tazobactam crystallization mother liquor to obtain the highest possible recovery rate of tazobactam.

7. The method for recovering products from tazobactam crystallization mother liquor by membrane process according to claim 6, characterized in that: The secondary crystallization mother liquor V is subjected to a continuous concentration operation method in which the secondary crystallization mother liquor V is subjected to multiple crystallization treatments to obtain multiple crystallization mother liquors, and then the multiple crystallization mother liquors are distilled to obtain ethanol and hazardous waste, and the ethanol is recycled.

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