CN112892229A - Virus composite filtering membrane and preparation method thereof - Google Patents
Virus composite filtering membrane and preparation method thereof Download PDFInfo
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- CN112892229A CN112892229A CN202110114248.0A CN202110114248A CN112892229A CN 112892229 A CN112892229 A CN 112892229A CN 202110114248 A CN202110114248 A CN 202110114248A CN 112892229 A CN112892229 A CN 112892229A
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a composite filtering membrane with a good separation effect and a preparation method thereof. The composite filtering membrane provided by the invention comprises a pre-filtering membrane, an ultrafiltration membrane and a middle supporting layer, wherein the aperture of the pre-filtering membrane is 50-1000 nm; the aperture of the small-hole ultrafiltration membrane is 10-20nm, and the preparation is completed by a two-step method. The pre-filtering membrane is made of one or more of cellulose acetate, regenerated cellulose, polyacrylonitrile, nylon and the like; the ultrafiltration membrane is made of one or more of polysulfone, polyethersulfone, polyvinyl chloride and polyvinylidene fluoride. Aiming at the problems that the flux of a conventional virus filtering membrane is low, the filtering requirement of a high-concentration biological medicine preparation cannot be met and the like, the composite filtering membrane provided by the invention is provided with a gradient micropore pre-filtering layer and a compact homogeneous ultrafiltration membrane layer, and can realize the rapid filtering of viruses, so that the production process requirement of the high-added-value biological medicine preparation is better met.
Description
Technical Field
The invention belongs to the technical field of filtering membranes, and particularly relates to a virus composite filtering membrane and a preparation method thereof.
Background
Viral filtration is a commonly occurring step in biopharmaceutical virus removal. The virus filtering membrane is widely used in the production of intravenous injection human immunoglobulin and monoclonal antibody due to high efficiency, low cost, environmental protection, easy realization and the like. The pore sizes of the virus filtration membranes commonly used at present are 50nm and 20 nm. 20nm is more commonly used because it is effective in trapping most viruses.
Viral filtration membranes need to be highly selective, and therefore often require the retention and permeation of viral and target protein products that differ in size by less than a factor of 2 during production use. The size of monoclonal antibodies is around 12nm, while the size of viruses is 20nm, with size differences of less than 2-fold. This requires that the viral filtration membrane must be precise in pore size and narrow in pore size distribution. At present, the organic membrane which realizes mass production can not meet the requirement of a virus filtering membrane in the aspect of precision, and has the problems of uneven pore size distribution, low reliability and the like. Therefore, in the field of virus filtration application, the precise distribution of the pore diameter is realized, and a huge benefit value space exists.
Chinese patent application publication No. CN111821535A discloses a virus filter tube for blood. The virus filtering tube for blood comprises a flow tube and a plurality of filtering membrane groups. The aperture of the filter membrane group is gradually reduced along the flow direction of the medium, various cells in the blood are separated step by step, and finally the quantity of the cytomegalovirus in the blood is reduced to be approximately equal to zero.
Chinese patent application No. CN111848784A discloses a method for separating and purifying high-concentration intravenous human immunoglobulin. Removing impurity proteins and coagulation factor substances by adopting a high-concentration urea solution pre-precipitation and octanoic acid precipitation method, and finally carrying out chromatography. The method can effectively reduce the content of IgA and polymer in human immunoglobulin for intravenous injection, and improve the purity.
Chinese patent application with patent publication No. CN101069750A discloses a virus-removing filter material made of porous fibers and a preparation method thereof. Comprises a prefiltration microporous membrane and a virus-removing microporous membrane compounded on the surface of the prefiltration microporous membrane. Can realize the separation efficiency of 99.99 percent for the virus with the size of more than 50 nm. The membrane preparation process is simple, but is not suitable for viruses with the size of 20nm which need to be separated in the monoclonal antibody production process.
Chinese patent application with patent publication No. CN110711493A discloses an HIV virus adsorption membrane and a preparation method thereof. The adsorption membrane material with the porous structure is mixed with lignin with positive charged particles, so that HIV virus can be effectively adsorbed.
The above patents all have specific environments or specific types of separable viruses, and have the disadvantages of low separation efficiency with a single aperture, complicated multi-stage separation process, and the like. At present, the preparation technology aiming at the high-efficiency virus filtration membrane required in the production process of the monoclonal antibody in China is still in a blank stage. Aiming at the problems that the conventional virus filtering membrane has low flux and cannot meet the filtering requirement of a high-concentration biological medicine preparation and the like, the invention aims to prepare the novel filtering membrane which has a multistage membrane pore structure and can rapidly filter viruses.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a virus composite filtering membrane with better separation effect and a preparation method thereof.
The invention provides a composite filtering membrane, which has a composite structure comprising a pre-filtering membrane, a middle supporting layer and a small-hole ultrafiltration membrane in sequence; the pore diameter of the pre-filtering membrane is 50-1000 nm; the aperture of the ultrafiltration membrane is 10-20 nm.
Preferably, the material of the pre-filtering membrane is one or more of cellulose acetate, regenerated cellulose, polyacrylonitrile, nylon and the like; the ultrafiltration membrane is made of one or more of polysulfone, polyethersulfone, polyvinyl chloride and polyvinylidene fluoride.
Preferably, the support layer is a non-woven fabric support layer, and the non-woven fabric is made of polyethylene terephthalate or polypropylene.
Preferably, the composite membrane is prepared by a two-step process, wherein the ultrafiltration membrane layer is firstly scraped on one side of the support layer, and then the prefiltration membrane layer is scraped on the other side of the post-treated support layer.
The invention also provides a preparation method of the composite filtering membrane, which comprises the following steps:
(1) adding a membrane preparation material, a solvent and an additive into a reaction kettle, dissolving and stirring at 20-100 ℃, respectively preparing a pre-filtration membrane and an ultrafiltration membrane preparation casting solution, and standing and defoaming for 4-12 hours for later use;
(2) starting a self-made continuous film scraping machine, controlling the film scraping temperature to be 25-70 ℃, the film scraping speed to be 0.5-2 m/min, and taking water as a coagulating bath;
(3) taking non-woven fabrics as a base material, adopting a self-made continuous film scraping machine, immersing a primary film with the thickness of 100-;
(4) taking the prepared small-hole ultrafiltration membrane as a substrate, scraping a pre-filtering layer with the thickness of 200-500 mu m on the other side of the non-woven fabric, evaporating, and immersing into a coagulating bath for curing to form a membrane to obtain a pre-filtering nascent composite membrane;
(5) and rinsing and airing the nascent composite membrane to obtain a finished product composite filtering membrane.
Preferably, the mass fraction of the film-making material is 8-18%, the mass fraction of the film-making solvent is 20-70%, and the mass fraction of the additive is 10-40%.
Preferably, the film-making solvent is one or a mixture of N-methyl pyrrolidone, dimethylformamide and dimethylacetamide; the additive comprises one or a mixture of more of polyethylene glycol, polymethyl pyrrolidone, glycerol, acetone, ethanol, isopropanol, n-butanol and n-octanol.
Preferably, when preparing the small-pore ultrafiltration membrane, the mass ratio of the membrane preparation material, the solvent and the additive is (10-25): (50-80): (10-20).
Preferably, when the pre-filtering membrane is prepared, the mass ratio of the membrane preparation material, the solvent and the additive is (5-20): (20-60): (20-50).
The composite filtering membrane prepared by the invention has a multi-stage membrane pore structure and high separation efficiency, and can realize rapid filtration of viruses, thereby better meeting the filtration requirements of high-concentration biological medicine preparations.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments of the invention, as illustrated in the accompanying drawings. Like reference numerals refer to like parts throughout the drawings, and the drawings are not intended to be drawn to scale in actual dimensions, emphasis instead being placed upon illustrating the principles of the invention.
FIG. 1 is a schematic cross-sectional structure diagram of an ultrafiltration membrane provided by the present invention.
FIG. 2 is a schematic view of the surface structure of a prefiltration membrane provided by the present invention.
Detailed Description
The technical solutions of the present invention are further described in detail with reference to specific examples so that those skilled in the art can better understand the present invention and can implement the present invention, but the examples are not intended to limit the present invention.
Referring to fig. 1 and 2, a composite filtering membrane is provided according to an embodiment of the present invention, and the composite structure of the composite filtering membrane is a pre-filtering membrane, a middle supporting layer, and a small-pore ultrafiltration membrane in sequence. The aperture of the pre-filtering membrane is 50-1000 nm; the pore diameter of the ultrafiltration membrane is 10-20 nm.
The composite filtering membrane provided by the invention is suitable for physically separating viruses in the field of biological manufacturing, and can be used as a virus filtering membrane. Passing through a 20nm ultrafiltration membrane and a prefiltration membrane of gradient pore structure. Before separating virus, large-particle impurities are effectively intercepted, so that the separation efficiency is further improved, and the problems of poor virus filtering effect, easiness in pollution and low membrane flux are solved. The virus filtering membrane prepared by the method has the advantages of good separation effect, high membrane flux, low cost and wide application range.
The composite filtering membrane provided by the invention has the advantages of reliable structure, difficult hole blockage, large membrane flux, high efficiency and the like through multi-stage separation. The virus can be accurately separated in the practical application environment, and the effective components are reserved.
The composite filtering membrane provided by the invention solves the problem of rapid and effective filtration of viruses in the production process of monoclonal antibodies. Impurities in the stock solution are classified and intercepted by a pre-filtering membrane, viruses are filtered and intercepted by an ultrafiltration membrane with accurately controlled aperture, and the problems of poor separation effect, low separation efficiency, complicated separation process and the like in the practical application process are solved by the form of a composite double-layer membrane.
The composite filtering membrane provided by the invention has the advantages of good separation effect, wide applicability and high selectivity, and can be applied to the biological field and other fields. Besides the environment which is very suitable for separating the virus by using the monoclonal antibody, the monoclonal antibody can also be applied to other environment systems with the particle size of about 20nm which needs to be separated.
In a preferred embodiment, the material of the pre-filtering membrane is one or more of cellulose acetate, regenerated cellulose, polyacrylonitrile, nylon and the like; the ultrafiltration membrane is made of one or more of polysulfone, polyethersulfone, polyvinyl chloride and polyvinylidene fluoride.
In a preferred embodiment, the support layer is a non-woven fabric support layer, and the non-woven fabric is made of polyethylene terephthalate or polypropylene.
In a preferred embodiment, the composite filtration membrane is prepared by a two-step process, wherein the ultrafiltration membrane layer is first scraped on one side of the support layer, and then the prefiltration membrane layer is scraped on the other side of the post-treated support layer.
The embodiment of the invention also provides a preparation method of the composite filtering membrane, which comprises the following steps:
(1) adding a membrane making material, a membrane making solvent and an additive into different reaction kettles according to a certain proportion to form a membrane casting material/solvent/additive ternary system, dissolving and stirring at 20-100 ℃, standing and defoaming for 4-24 hours, and respectively preparing an ultrafiltration membrane and a pre-filtration membrane casting solution; the ultrafiltration membrane system is preferably dissolved and stirred at 50-80 ℃, then kept stand and defoamed for 5-20 hours, the pre-filtration membrane is preferably dissolved and stirred at 25-50 ℃, and then kept stand and defoamed for 4-12 hours;
(2) starting a continuous film scraping machine, and controlling the temperature of a film scraping area to be 25-70 ℃;
(3) regulating and controlling the film scraping speed to be 0.5-2 m/min, taking water as a coagulating bath, taking non-woven fabric as a base material, adopting a self-made continuous film scraping machine, dipping a primary film into the coagulating bath to solidify and form a film to obtain a small-hole ultrafiltration film, rinsing and the like, and then airing for later use.
(4) And (3) scraping the membrane on the other side of the non-woven fabric by using a self-made membrane scraping machine on the basis of the prepared ultrafiltration membrane, wherein the thickness of the membrane is 200-500 mu m, and the membrane is subjected to evaporation treatment and then is immersed into a coagulating bath to be solidified into a membrane to obtain a pre-filtering layer.
(5) The separation membrane prepared by the two-step method is subjected to post-treatment processes such as rinsing, natural airing and the like to obtain the composite filtering membrane.
In a preferred embodiment, the mass fraction of the film-making material is 8% -18%, the mass fraction of the film-making solvent is 20% -70%, and the mass fraction of the additive is 10% -40%.
In a preferred embodiment, the film-making solvent is one or a mixture of N-methyl pyrrolidone, dimethylformamide and dimethylacetamide; the additive comprises one or more of polyethylene glycol, polymethyl pyrrolidone, glycerol, acetone, ethanol, isopropanol, n-butanol and n-octanol.
In the preferred embodiment, in the step (4), the temperature of the evaporation environment is 30-100 ℃, the relative humidity is 50-100%, and the time is controlled within 120 seconds.
In a preferred embodiment, when the ultrafiltration membrane is prepared, the mass ratio of the membrane preparation material, the solvent and the additive is (10-25): (50-80): (10-20); when the pre-filtering membrane is prepared, the mass ratio of the membrane preparation material, the solvent and the additive is (5-20): (20-60): (20-50).
The preparation method of the composite filtering membrane provided by the invention takes one or more of cellulose acetate, regenerated cellulose, polyacrylonitrile, nylon and the like as a membrane making material of the pre-filtering membrane; one or more of polysulfone, polyethersulfone, polyvinyl chloride and polyvinylidene fluoride are used as ultrafiltration membrane making materials, dimethylformamide and/or dimethylacetamide is used as a mixed solvent system, acetone, glycerol and the like are used as non-solvent additives and plasticizers, and an uniform-pore ultrafiltration membrane and a gradient-pore prefiltration membrane are respectively prepared on two sides of a non-woven fabric. After the membrane is scraped, under the control condition of specific temperature and humidity, the structure of the membrane pores is adjusted through pre-volatilization treatment, and then the membrane is immersed into a coagulating bath, so that the membrane is completely solidified and all the solvent is exchanged. The virus filtering membrane in the form is subjected to multi-stage separation, has a reliable structure, and has the advantages of difficult pore blocking, large membrane flux, high efficiency and the like. Can accurately filter viruses in practical application environment and keep effective components.
In order to further understand and appreciate the technical solution of the present invention, the embodiments are now described in further detail.
Example 1
Preparing an uniform-pore ultrafiltration membrane:
the polyether sulfone, the dimethylformamide, the polymethyl pyrrolidone and the glycerol are mixed according to the mass ratio of 20:65:10:5, stirred for 12 hours at the temperature of 60 ℃ to prepare a clear and transparent solution, and the clear solution is kept still for defoaming. And starting the continuous film scraping machine to uniformly scrape the casting film liquid on the non-woven fabric, and collecting the casting film liquid into a coil after passing through a coagulating bath. Referring to fig. 1, it can be observed that the pore size of the prepared ultrafiltration membrane is uniformly dense.
Preparing a gradient hole prefiltration membrane:
the method comprises the steps of mixing and putting a mixture of dimethyl cellulose, dimethyl formamide, acetone and glycerol into a continuous film scraping machine kettle body according to the mass ratio of 10:50:20:20, stirring at normal temperature for 12 hours to prepare a clear transparent solution, and standing for defoaming. And starting a continuous film scraping machine, uniformly coating the membrane casting solution on the other side of the non-woven fabric on the basis of preparing the ultrafiltration membrane, pre-evaporating for 60 seconds under the environmental condition of 70 ℃, and then curing the primary membrane into a membrane through a coagulating bath. Referring to fig. 2, it can be observed that the surface of the prepared pre-filtering membrane is of a macroporous structure, so that large-particle impurities can be effectively intercepted, and the separation efficiency is further improved.
The composite filtering membrane provided by the embodiment has a good separation effect when being applied to separation of high-concentration biological medicine preparations. The gradient pore pre-filtering membrane can effectively intercept large particle impurities and avoid blockage of the small pore ultrafiltration membrane, so that efficient and accurate filtration of viruses is better realized.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A composite filtering membrane is characterized in that a composite structure of the composite filtering membrane is sequentially a pre-filtering membrane, a middle supporting layer and a small-hole ultrafiltration membrane; the pore diameter of the pre-filtering membrane is 50-1000 nm; the aperture of the ultrafiltration membrane is 10-20 nm.
2. The composite filtering membrane according to claim 1, wherein the pre-filtering membrane is made of one or more of cellulose acetate, regenerated cellulose, polyacrylonitrile, nylon and the like; the ultrafiltration membrane is made of one or more of polysulfone, polyethersulfone, polyvinyl chloride and polyvinylidene fluoride.
3. The composite filtration membrane of claim 1, wherein the support layer is a non-woven fabric support layer, and the non-woven fabric is made of polyethylene terephthalate or polypropylene.
4. The composite filtration membrane of claim 1, wherein said composite filtration membrane is prepared using a two-step process, first scraping the ultrafiltration membrane layer on one side of the support layer and then scraping the prefiltration membrane layer on the other side of the post-treated support layer.
5. The preparation method of the composite filtering membrane is characterized by comprising the following steps of:
(1) adding a membrane preparation material, a solvent and an additive into a reaction kettle, dissolving and stirring at 20-100 ℃, respectively preparing a pre-filtration membrane and an ultrafiltration membrane preparation casting solution, and standing and defoaming for 4-12 hours for later use;
(2) starting a self-made continuous film scraping machine, controlling the film scraping temperature to be 25-70 ℃, the film scraping speed to be 0.5-2 m/min, and taking water as a coagulating bath;
(3) taking non-woven fabrics as a base material, adopting a self-made continuous film scraping machine, immersing a primary film with the thickness of 100-; regulating and controlling the evaporation temperature of a film scraping machine to be 50-100 ℃, the humidity to be 50-95RH percent and the evaporation time to be 10-120 s;
(4) taking the prepared small-hole ultrafiltration membrane as a substrate, scraping a pre-filtering layer with the thickness of 200-500 mu m on the other side of the non-woven fabric, evaporating, and immersing into a coagulating bath for curing to form a membrane to obtain a pre-filtering nascent composite membrane;
(5) and rinsing and airing the nascent composite membrane to obtain a finished product composite filtering membrane.
6. The method for producing a composite filtration membrane according to claim 5, wherein the mass fraction of the membrane-forming material is 8% to 18%, the mass fraction of the membrane-forming solvent is 20% to 70%, and the mass fraction of the additive is 10% to 40%.
7. The method for preparing the composite filtration membrane according to claim 5, wherein the membrane-forming solvent is one or a mixture of N-methylpyrrolidone, dimethylformamide and dimethylacetamide; the additive comprises one or a mixture of more of polyethylene glycol, polymethyl pyrrolidone, glycerol, acetone, ethanol, isopropanol, n-butanol and n-octanol.
8. The production method of the composite filtration membrane according to claim 5, wherein when the small-pore ultrafiltration membrane is produced, the mass ratio of the membrane-making material, the solvent and the additive is (10-25): (50-80): (10-20).
9. The production method of the composite filtration membrane according to claim 5, wherein when the prefiltration membrane is produced, the mass ratio of the membrane-forming material, the solvent and the additive is (5-20): (20-60): (20-50).
10. The method for preparing a composite filtration membrane according to claim 5, wherein in the step (4), the temperature of the evaporation environment is 30 ℃ to 100 ℃, the relative humidity is 50% to 100%, and the time is controlled within 120 seconds.
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