Preparation method of steam-sterilization-resistant hollow fiber membrane module

Abstract

The invention relates to the technical field of membrane separation, in particular to a preparation method of a steam-sterilization-resistant hollow fiber membrane component, which is used for preparing a hollow fiber membrane capable of resisting moist heat steam sterilization at 121 DEG C, and the membrane can resist moist heat sterilization under the pressure of 2bar. The preparation method comprises the following steps: bundling the hollow fiber membrane filaments and loading the hollow fiber membrane filaments into a membrane shell, selecting a steam-resistant sterilization type hollow fiber membrane as the hollow fiber membrane filaments, selecting a polysulfone material as the membrane shell material, and then preparing the hollow fiber membrane module by using epoxy resin pouring sealant through centrifugal casting, and the module can be applied to the field of medicine. According to the preparation method of the steam-sterilization-resistant hollow fiber membrane module, the epoxy resin pouring sealant is subjected to the steps of centrifugal pouring, hollow fiber membrane module assembling treatment and hollow fiber membrane module post-treatment, so that high-temperature steam sterilization treatment can be carried out in an environment of 121 DEG C, and the requirements of cell perfusion culture and virus removal are met; therefore, the pharmaceutical process is more effectively applied.

Description

Technical Field

[0001] The invention relates to the technical field of membrane separation, in particular to a method for preparing a steam sterilization-resistant hollow fiber membrane component. Background Art

[0002] Membrane separation technology utilizes the differences in the selective permeability of membrane pores to each component to achieve separation and purification of solvents and solutes in the components. According to the size of the retention pores, it can be divided into microfiltration membranes, ultrafiltration membranes, nanofiltration membranes and reverse osmosis membranes, etc. According to the form of membrane components, it can be divided into hollow fiber membranes, spiral membranes, tubular membranes, etc. The essential filtration mechanism of microfiltration membrane is screening and retention, and its effective pore size range is 0.1-10μm. The membrane has a small thickness, large pore size, high porosity, large flux, and low membrane adsorption pollution. It can effectively retain solid particles, organic colloids, some bacteria and other impurities in the gas and liquid phases under a pressure of 0.1-0.3Mpa. It is mainly used in water purification, juice concentration, battery separators, pharmaceutical sterilization and suspended solids and other fields; compared with microfiltration membranes, ultrafiltration membranes have smaller pore sizes and require a higher pressure difference as the driving force of the membrane process. It has higher pressure and smaller flux. It mainly retains large molecules, small-sized particles, colloids, viruses, etc. It is mainly used in protein concentration and recovery, antibiotic separation, drinking water purification, electrophoretic paint recovery, seawater desalination pretreatment and other fields. Nanofiltration membrane is a polymer membrane with a pore size of about 1nm. It is a new type of membrane separation technology that has developed rapidly in the world in recent years. It has the ability to partially intercept monovalent ions and completely intercept multivalent ions. Due to its low operating pressure, it can also retain minerals beneficial to the human body after filtration. In the field of water purification in recent years, it has been valued by researchers and end users. Compared with reverse osmosis, nanofiltration membrane and nanofiltration technology have the characteristics of easy operation, low maintenance cost, low energy consumption, high flux, etc., and have been applied in the fields of food and chemical industry, sewage treatment, pharmaceutical industry, desalination industry, etc.

[0003] In the field of medicine, especially biopharmaceuticals, hollow fiber membranes are widely used due to their precise separation accuracy, relatively mild use conditions, no phase change during use, ultra-low shear force, and completely sealed use conditions. The membrane separation process accounts for nearly half of the biopharmaceutical process. However, in most pharmaceutical processes, such as cell perfusion culture and virus removal processes, the components need to be sterilized with 121°C high-temperature steam to meet the use requirements; in view of this, we proposed a method for preparing a steam sterilization-resistant hollow fiber membrane component. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a method for preparing a steam sterilization-resistant hollow fiber membrane module, which solves the problems mentioned in the above background technology.

[0005] To achieve the above objectives, the present invention is implemented by the following technical scheme: a method for preparing a steam sterilization resistant hollow fiber membrane module, the method comprising the following steps: S1, packing the hollow fiber membrane bundle into the membrane shell; S2, preparing a hollow fiber membrane assembly by centrifugal casting with epoxy resin potting glue; S3, post-processing the cast membrane assembly to make it meet the requirements of 121°C steam sterilization; S4, hollow fiber membrane assembly processing; S5, post-processing of hollow fiber membrane modules; S6. Steam sterilization validation.

[0006] Optionally, the hollow fiber membrane is a steam sterilization-resistant hollow fiber membrane, and the membrane pore size ranges from 2nm to 650nm.

[0007] Optionally, the membrane shell material is polysulfone, and the membrane shell joint needs to be grooved and stabilized.

[0008] Optionally, the epoxy resin is an epoxy resin resistant to high-temperature steam at 121°C.

[0009] Optionally, the special post-treatment method is to cure at a constant temperature of 80° C. for 4 to 12 hours.

[0010] Optionally, the S4 includes: S41, fiber bundle preparation: cutting the prepared hollow fiber membrane into a suitable length, and then neatly bundling multiple hollow fiber membranes into a bundle, ensuring that both ends of the fiber bundle are flat; S42, loading into the housing: putting the fiber bundle into the pre-prepared component housing, the housing is made of corrosion-resistant and high-temperature-resistant materials, and the two ends of the fiber bundle should be aligned with the interface of the housing for subsequent sealing and connection; The material of the shell is one of stainless steel and polyolefin.

[0011] S43, Sealing and fixing: Use high temperature resistant and chemical corrosion resistant sealing materials to seal and fix the interface between the fiber bundle and the shell to ensure that no leakage occurs during steam sterilization and use. The sealing methods used include potting and gluing; the sealing material is one of silicone rubber and polytetrafluoroethylene.

[0012] Optionally, the S5 further includes: S51, cleaning: thoroughly clean the assembled membrane assembly with deionized water or other suitable solvents to remove possible residual impurities, solvents and unreacted substances to ensure the cleanliness of the membrane assembly; S52, Drying: Use room temperature drying or low temperature vacuum drying to dry the cleaned membrane components to a suitable moisture content to avoid excessive moisture affecting the sterilization effect or causing damage to the membrane components during steam sterilization; S53. Testing: Conduct performance tests on the prepared steam sterilization resistant hollow fiber membrane components, including gas flux, bubble point pressure, pore size distribution, and mechanical strength index testing to ensure that the membrane components meet the use requirements.

[0013] Optionally, the S6 further includes: Place the membrane assembly into the steam sterilization equipment and perform sterilization operations according to the set sterilization conditions; after the sterilization is completed, perform appearance inspection and performance test on the membrane assembly to verify whether the membrane assembly can still maintain good performance and structural integrity after steam sterilization; The sterilization conditions include: temperature 121° C., pressure 103.4 kPa, and time 15-30 minutes.

[0014] The present invention provides a method for preparing a steam sterilization-resistant hollow fiber membrane module, which has the following beneficial effects: The preparation method of the steam sterilization-resistant hollow fiber membrane component can meet the requirements of high-temperature steam sterilization treatment in an environment of 121° C., cell perfusion culture, and virus removal, by using epoxy resin potting glue through centrifugal casting, hollow fiber membrane component assembly processing, and hollow fiber membrane component post-processing steps, thereby more effectively utilizing the pharmaceutical process. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the process structure of the present invention. DETAILED DESCRIPTION

[0016] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.

[0017] The present invention provides a technical solution: a method for preparing a steam sterilization-resistant hollow fiber membrane component.

[0018] Embodiment 1: 1. Preparation of membrane components 1000 300cm hollow fiber membranes were assembled into the membrane shell, and the two-component epoxy resin potting glue was mixed with A:B100:50. The membrane was centrifuged and stirred at 50°C for 12 hours, the cut ends were removed, and then aged at 80°C for 4 hours. 2. Steam sterilization experiment The prepared membrane module was sterilized 10 times using an electric steam generator, with a steam temperature of 121°C and a steam pressure of 1.6 bar. The results were compared using diffusion flow data before and after the experiment. The experimental results are as follows: Embodiment 2: 1. Preparation of membrane components: 1000 300cm hollow fiber membranes were assembled into the membrane shell, and the two-component epoxy resin potting glue was mixed with A:B100:40. The mixture was centrifuged and stirred at 50℃ for 12 hours, the cut ends were removed, and then aged at 80℃ for 8 hours. 2. Steam sterilization experiment: The prepared membrane module was sterilized 10 times using an electric steam generator, with a steam temperature of 121°C and a steam pressure of 1.6 bar. The results were compared using diffusion flow data before and after the experiment. The experimental results are as follows: Embodiment 3: 1. Preparation of membrane components 5000 600cm hollow fiber membranes were assembled into the membrane shell, and the two-component epoxy resin potting glue was mixed in the ratio of A:B100:40. The membrane was centrifuged and stirred at 50°C for 8 hours, the cut ends were removed, and then aged at 80°C for 12 hours. 2. Steam sterilization experiment The prepared membrane module was sterilized 10 times using an electric steam generator, with a steam temperature of 121°C and a steam pressure of 1.6 bar. The results were compared using diffusion flow data before and after the experiment. The experimental results are as follows: As an application of this embodiment: by using epoxy resin potting glue through centrifugal casting, hollow fiber membrane component assembly processing and hollow fiber membrane component post-processing steps, it can meet the requirements of high-temperature steam sterilization at 121°C, achieve cell perfusion culture and virus removal, thereby more effectively utilizing the pharmaceutical process.

[0019] 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 preparing a steam sterilization-resistant hollow fiber membrane module, characterized in that The method comprises the following steps: S1, packing the hollow fiber membrane bundle into the membrane shell; S2, preparing a hollow fiber membrane assembly by centrifugal casting with epoxy resin potting glue; S3, post-processing the cast membrane assembly to make it meet the requirements of 121°C steam sterilization; S4, hollow fiber membrane assembly processing; S5, post-processing of hollow fiber membrane modules; S6. Steam sterilization validation.

2. A method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The hollow fiber membrane is a steam sterilization-resistant hollow fiber membrane, and the membrane pore size ranges from 2nm to 650nm.

3. A method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The membrane shell material is polysulfone, and the membrane shell joint needs to be modified for groove stabilization.

4. A method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The epoxy resin is an epoxy resin resistant to 121° C. high-temperature steam.

5. The method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The special post-treatment method is to cure at a constant temperature of 80° C. for 4 to 12 hours.

6. A method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The S4 includes: S41, fiber bundle preparation: cutting the prepared hollow fiber membrane into a suitable length, and then neatly bundling multiple hollow fiber membranes into a bundle, ensuring that both ends of the fiber bundle are flat; S42, loading into the housing: putting the fiber bundle into the pre-prepared component housing, the housing is made of corrosion-resistant and high-temperature-resistant materials, and the two ends of the fiber bundle should be aligned with the interface of the housing for subsequent sealing and connection; The material of the shell is one of stainless steel and polyolefin. S43, Sealing and fixing: Use high temperature resistant and chemical corrosion resistant sealing materials to seal and fix the interface between the fiber bundle and the shell to ensure that no leakage occurs during steam sterilization and use. The sealing methods used include potting and gluing; the sealing material is one of silicone rubber and polytetrafluoroethylene.

7. A method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The S5 further comprises: S51, cleaning: thoroughly clean the assembled membrane assembly with deionized water or other suitable solvents to remove possible residual impurities, solvents and unreacted substances to ensure the cleanliness of the membrane assembly; S52, Drying: Use room temperature drying or low temperature vacuum drying to dry the cleaned membrane components to a suitable moisture content to avoid excessive moisture affecting the sterilization effect or causing damage to the membrane components during steam sterilization; S53. Testing: Conduct performance tests on the prepared steam sterilization resistant hollow fiber membrane components, including gas flux, bubble point pressure, pore size distribution, and mechanical strength index testing to ensure that the membrane components meet the use requirements.

8. The method for preparing a steam sterilization resistant hollow fiber membrane module according to claim 1, characterized in that: The S6 further comprises: Place the membrane assembly into the steam sterilization equipment and perform sterilization operations according to the set sterilization conditions; after the sterilization is completed, perform appearance inspection and performance test on the membrane assembly to verify whether the membrane assembly can still maintain good performance and structural integrity after steam sterilization; The sterilization conditions include: temperature 121° C., pressure 103.4 kPa, and time 15-30 minutes.

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