CN114307650B - Sulfone polymer microporous liquid-stopping film and preparation method and application thereof - Google Patents

Abstract

The invention relates to a sulfone polymer microporous liquid-stopping film, a preparation method and application thereof, wherein the microporous liquid-stopping film comprises a first porous surface, a second porous surface and a porous main body positioned between the first porous surface and the second porous surface; the porous main body is internally provided with a non-directional tortuous path, and is characterized in that a sulfone polymer micropore liquid stopping film is used for stopping injection liquid containing plant extract liquid; in the sulfone polymer microporous liquid-stopping film, the ratio of the number of holes with the aperture not exceeding 2.5 mu m measured by a PMI aperture tester to the total number of holes is less than 10%; the porosity of the microporous liquid-stopping film of the sulfone polymer is at least 60%; the water BP value of the microporous liquid stopping film of the sulfone polymer is 20-50KPa, and the liquid stopping height is at least 1m. The sulfone polymer microporous liquid-stopping film provided by the technical scheme of the invention has more optimized film body structure and comprehensive performance, and has the advantages of large flux, stable flux, high filtering precision, excellent and stable liquid-stopping performance and higher applicability when being applied to liquid-stopping of Chinese patent medicines.

Description

Sulfone polymer microporous liquid-stopping film and preparation method and application thereof

Technical Field

The invention relates to the technical field of liquid-stopping film materials, in particular to a microporous liquid-stopping film of sulfone polymer and a preparation method and application thereof.

Background

An automatic liquid stopping infusion apparatus (Airstop, also called as self-drip stop, self-closing and anti-emptying infusion apparatus) is a novel disposable medical consumable material for replacing a common infusion apparatus, and has the functions of keeping the liquid level at a designated position for a long time without descending when the infusion process is finished, and automatically avoiding air from entering veins, thereby reducing the working pressure of nursing staff and psychological pressure of patients.

In recent years, automatic liquid-stopping infusion sets have been widely popularized in European and American regions and gradually popularized in China. When the infusion process is about to end and the liquid level drops to the liquid stopping film, the subsequent air can be blocked by the liquid stopping film and cannot enter the lower guide pipe continuously, and the liquid column in the lower guide pipe reaches an equilibrium state under the gravity, the atmospheric pressure, the venous pressure of a human body and the upward attractive force generated by the liquid stopping film, so that the automatic liquid stopping is realized.

The existing domestic drops are generally western medicine drops and Chinese patent medicine drops, the Chinese patent medicine is a type of Chinese medicine preparation which is prepared into a certain dosage form by processing the Chinese patent medicine drops according to a specified prescription and preparation process under the guidance of Chinese medicine theory and is approved by the national medicine supervision and management department for commercialization in order to prevent and treat diseases; such as SHENMAI injection, carthami flos injection, QINGKAILING injection, etc., has more large granule substances than western medicine drop system environment.

Therefore, when the liquid stopping film is used for stopping liquid in Chinese patent medicine drops, higher requirements are put on the flux and stability of the liquid stopping film, the liquid stopping height, the filtering precision and other comprehensive performances; when PES is used as a liquid stopping film of the Chinese patent medicine, the PES film is required to have larger flux, and the flux is stable, because the viscosity and the density of the Chinese patent medicine are higher than those of western medicines, and the Chinese patent medicine contains more large-particle substances, wherein the large-particle substances are usually glass-broken residues broken at the bottle mouth of an ampoule bottle, part of effective components in the liquid medicine of the Chinese patent medicine and the like, and when the liquid medicine is infused for a long time, the large-particle substances trapped in the liquid stopping film are continuously increased, so that the liquid medicine is not beneficial to pass through, the flux of a diaphragm is reduced, and the infusion speed is reduced, so that the infusion time is overlong, and discomfort of a patient can be caused; in addition, there are the following problems:

1. because the flux of the membrane is smaller, the Chinese patent medicine liquid is usually extracted from plants, so that the viscosity and density of the Chinese patent medicine are higher than those of western medicine prepared by solvent, and after the Chinese patent medicine liquid passes through the membrane, the Chinese patent medicine and part of active ingredients thereof can remain in the membrane, so that the curative effect of a patient is reduced, and the influence on the human health is caused.

2. Because the flux of the membrane is unstable, after a certain period of transfusion, the flux of the membrane can be quickly attenuated, so that the flux of the membrane is reduced, the transfusion speed is reduced, and the transfusion time is too long, so that discomfort of a patient can be caused.

Disclosure of Invention

Aiming at the defects existing in the prior art, the invention aims to provide a sulfone polymer microporous liquid-stopping film which is applied to Chinese patent medicine drip, has large flux and stability and excellent comprehensive performance, and a method for preparing the sulfone polymer microporous liquid-stopping film, so as to solve the problems of small flux, unstable flux and poor comprehensive performance of the existing liquid-stopping film.

In order to achieve the above purpose, the invention adopts the following technical scheme:

a sulfone polymer microporous liquid-stopping film comprising a first porous surface, a second porous surface, and a porous body positioned between the first porous surface and the second porous surface, the porous body having a non-directional tortuous path therein, the sulfone polymer microporous liquid-stopping film being for stopping an injection liquid comprising a botanical extract;

in the sulfone polymer microporous liquid-stopping film, the ratio of the number of holes with the aperture not exceeding 2.5 mu m measured by a PMI aperture tester to the total number of holes is less than 10%;

the porosity of the microporous liquid-stopping film of the sulfone polymer is at least 60%;

the water BP value of the microporous liquid stopping film of the sulfone polymer is 20-50KPa, and the liquid stopping height is at least 1m.

The sulfone polymer microporous liquid stopping film provided by the invention is used for stopping injection liquid containing plant extract liquid, and is particularly suitable for being applied to injection liquid containing plant extract liquid with the density of more than 1.02g/cm ³ And a viscosity greater than 1.25 cps; wherein, the plant extract can be understood as Chinese medicinal liquid, such as SHENMAI injection, HONGHUA injection, QINGKAILING injection, etc.; the density and viscosity of the Chinese patent medicine liquid are generally higher than those of the western medicine liquid, and large granular substances (effective components of the Chinese patent medicine, broken glass slag at the mouth of an ampoule bottle and the like) are more in an environment system of the Chinese patent medicine liquid, and it is understood that when the Chinese patent medicine liquid passes through the membrane, part of the large granular substances can block holes of the membrane, so that the flux of the membrane decays too fast; because the density and viscosity of the Chinese medicinal liquid are both larger than those of the western medicinal liquid, that is, the friction force between the Chinese medicinal liquid and the membrane is larger than that between the western medicinal liquid and the membrane, the flux of the Chinese medicinal liquid between the membranes is smaller than that of the western medicinal liquid, so as to ensure the delivery of patientsThe liquid-time comfort level is high, and the sulfone polymer microporous liquid-stopping film has large flux, so that the flux of the film is not reduced due to the large density and viscosity of the liquid medicine when the Chinese patent medicine liquid passes through the sulfone polymer liquid-stopping film; the flux of the microporous liquid-stopping film of the sulfone polymer is stable, namely, the Chinese patent medicine liquid passing through the film is increased along with the increase of the infusion time, and the flux attenuation of the film is slow; in the microporous liquid-stopping film of the sulfone polymer, the ratio of the number of holes with the diameter of not more than 2.5 mu m passing through a PMI aperture tester to the whole number of holes is less than 10%, preferably 3-8%, wherein the holes with the diameter of not more than 2.5 mu m measured by the PMI are defined as small holes, the ratio of the number of the small holes to the whole number of the holes cannot be excessively large, otherwise, the smaller the number of the small holes is, the more the passage of the Chinese patent medicine liquid through the membrane is narrower, the smaller the flux in unit time is, the more large granular substances are contained in the Chinese patent medicine liquid, and when the large granular substances are generally prepared by the Chinese patent medicine, the bottleneck glass slag of an ampoule bottle falls into the liquid medicine, the particle size of the granular substances is larger, and when the number of the small holes is larger, the granular substances block more small holes, so that the flux of the Chinese patent medicine liquid medicine in unit time is reduced, even the Chinese patent medicine liquid cannot pass through the membrane, and the infusion time of a patient is prolonged, and physical discomfort and psychological anxiety of the patient are caused; meanwhile, the ratio of the small holes to the whole holes cannot be too small, the small holes ensure that the Chinese patent medicine liquid and the membrane have larger surface tension, the capillary phenomenon generated when the Chinese patent medicine liquid enters the membrane is strong, the membrane is ensured to realize liquid stopping, and the liquid stopping height is at least 1m; and when the number of the small holes is too small, the filtering precision of the membrane is reduced.

The pore rate refers to the proportion of the membrane pore volume of the liquid stopping membrane to the total volume, the sulfone polymer microporous liquid stopping membrane is formed by sequentially arranging a first porous surface, a porous main body and a second porous surface along the thickness direction, wherein the porous main body is internally provided with a non-directional tortuous path, the non-directional tortuous path refers to a randomly-oriented groove structure and/or a discretely-distributed hole structure, the non-directional tortuous paths are mutually communicated, the liquid medicine flows in from the second porous surface, flows out from the first porous surface after flowing through the path, the proportion of the volumes of the groove structure and the hole structure to the total volume of the membrane is at least 60%, preferably more than 70%, and when the membrane is completely wetted by Chinese patent medicine liquid medicine, the proportion of the Chinese patent medicine liquid medicine in the membrane is at least 70%, namely the volume of the Chinese patent medicine liquid medicine passing through the membrane in unit time is larger, and the higher porosity further ensures that the sulfone polymer microporous liquid stopping membrane has higher flux.

The PMI aperture tester is CFP-1J00AEX, and uses a gas-liquid and liquid-liquid discharge method to measure the aperture distribution of the microporous liquid-stopping film of the sulfone polymer; or the film section structure is calculated and measured by using computer software (such as Matlab, NIS-Elements and the like) or manually after the appearance of the film section structure is represented by using a scanning electron microscope; of course, the person skilled in the art can also obtain the above parameters by other measuring means, which are only used as reference.

The microporous liquid-stopping film of the sulfone polymer provided by the invention has good liquid-stopping performance, and has high and stable liquid-stopping height and no reflux; preferably, the liquid-stopping height of the membrane is more than 1.5 m; the sulfone polymer microporous liquid stopping film generates surface tension with the Chinese patent medicine liquid medicine to balance the hydrostatic pressure of the liquid medicine between the sulfone polymer microporous liquid stopping film and the needle head, so that liquid stopping is realized, when the Chinese patent medicine liquid medicine wets the sulfone polymer microporous liquid stopping film, capillary phenomenon is generated inside the film, and the critical pressure of the gas passing through the wetted film is called as BP value, so that the BP value and the liquid stopping height are positively correlated, and the higher the BP value is, the higher the liquid stopping height is.

Preferably, the negative charge density per unit area of the microporous liquid-stop film of the sulfone polymer is not more than 70 x 10 ^-9 mol/cm ² Preferably (20-55) ×10 ^-9 mol/cm ² The method comprises the steps of carrying out a first treatment on the surface of the The unit mass negative charge density of the microporous liquid-stopping film of the sulfone polymer is not more than 150 x 10 ≡ ^-10 mol/mg。

The unit area negative charge density of the microporous liquid-stopping film of the sulfone polymer is preferably (30-40) 10 ≡ ^-9 mol/cm ² The negative charge density per unit mass is preferably (70-100) 10 ≡ ^-10 mol/mg; it can be understood that the specific surface area of the microporous liquid-stopping film of the sulfone polymer cannot be too large, namely the contact area between the microporous liquid-stopping film and the membrane is not too large when the liquid medicine of the Chinese patent medicine passes through the membrane, the greater the negative charge density is, the stronger the adsorption capacity of the membrane is, the density and viscosity of the liquid medicine are larger when the liquid medicine of the Chinese patent medicine passes through the membrane, the time of passing the liquid medicine through the membrane is longer, namely the residence time of the liquid medicine in the membrane is longer, so that the effective components in the liquid medicine are easy to be absorbed by the membrane, the absorption of the medicine by a patient is not facilitated, meanwhile, after a large amount of effective components are adsorbed in the membrane, the drug effect is reduced, the recovery of the patient is not facilitated, and the porosity of the membrane is reduced, so that the flux of the membrane is reduced too fast, the transfusion time is too long, and discomfort of the patient is easy to be caused after long transfusion. For example, the negative charges are hydroxyl groups, sulfonic acid groups and the like, wherein the number of the hydroxyl groups and the hydrophilicity of the membrane are positively correlated, for example, in a similar ginseng-malt injection, the saponin substances are regarded as effective drug components, the structural formula of the substances contains more hydroxyl groups, the hydroxyl groups are ionized to enable the saponin substances to have weak electronegativity, and when the negative charge density of the membrane is more than 20 x 10 ≡ ^-9 mol/cm ² Can ensure the hydrophilicity of the membrane, i.e. the membrane can be wetted rapidly when the negative charge density of the membrane is less than 55 x 10 ^-9 mol/cm ² In this case, the adsorption of the active ingredients in the Chinese medicinal liquid by the membrane can be reduced, and the therapeutic effect of the liquid can be ensured. In addition, as the pore diameter of the membrane is smaller, the specific surface area of the membrane is larger, and therefore, the pore diameter in the membrane cannot be too large or too small, and a suitable pore is required.

Preferably, in the microporous liquid-stopping film of the sulfone polymer, the ratio of the number of holes with the aperture exceeding 6 μm measured by the PMI aperture tester to the total number of holes is 1-12%.

The holes with the pore diameter exceeding 6 mu m measured by PMI are defined as macropores, the ratio of the macropores to the holes is not excessively large, preferably 3-9%, otherwise, the larger the macropores are, the larger the number is, firstly, the smaller the surface tension between the Chinese patent medicine liquid medicine and the membrane is, and the weaker the capillary phenomenon generated when the liquid medicine passes through the membrane is, so that the liquid stopping height of the membrane is lower or the liquid stopping is not possible, and the applicability is not realized; secondly, the larger the pore diameter of the macropores is, the larger the number is, and the filtration performance of the membrane can be reduced; in addition, when the Chinese patent medicine liquid is stopped, the fact that large granular substances exist in the Chinese patent medicine liquid, such as glass slag and the like at the broken part of the bottle mouth of an ampoule bottle, and the large holes can cause the glass slag to be not completely trapped, so that certain potential safety hazards exist after the large granular substances such as glass slag flow into a human body along with the liquid medicine, and in addition, the liquid stopping performance of a film can be influenced; meanwhile, the ratio of the large holes to the whole holes cannot be too small, the flux of the membrane is reduced when the large holes are small, the flow speed of the liquid medicine is reduced after passing through the membrane, the transfusion time of a patient is prolonged, the flux attenuation speed of the membrane is high along with the time, the flow speed of the liquid medicine in the transfusion process is unstable, and the situation of being slower and slower can occur, so that discomfort or psychological anxiety of the patient is caused.

The holes with the aperture of 2.5-6 mu m measured by PMI are defined as mesopores, the ratio of the number of the mesopores to the number of the holes is preferably 85-95%, and excessive holes with the aperture of more than 6 mu m measured by PMI easily cause large particle impurities in the Chinese patent medicine liquid, such as glass slag, to easily pass through, reduce the filtering precision of the membrane and have potential safety hazards to human health; thus, holes with a pore diameter exceeding 6 μm as measured by PMI cannot occupy too large a ratio; holes with the diameter smaller than 2.5 mu m are measured by the PMI, so that the flux of the liquid medicine in unit time is smaller, particularly the density and viscosity of the Chinese patent medicine liquid are larger, the circulation of the Chinese patent medicine liquid is more unfavorable, and glass slag can be blocked after the liquid medicine passes through the holes, so that the flux of a membrane is reduced, the circulation of the liquid medicine is unfavorable, and the flow rate of the liquid medicine is influenced, therefore, the holes with the diameter smaller than 2.5 mu m are measured by the PMI and cannot occupy too large proportion; the holes with the aperture of 2.5-6 mu m measured by the PMI can ensure the filtering precision of the membrane, and can ensure the slow flux attenuation of the membrane along with the extension of infusion time.

Preferably, the first porous surface is provided with a plurality of first holes, and the average pore diameter of the first holes is 4-20 mu m;

The second porous surface is provided with a plurality of second holes, and the average pore diameter of the second holes is 7-28 mu m.

The second porous surface is used as the liquid inlet surface of the Chinese patent medicine liquid, the first porous surface is used as the liquid outlet surface of the Chinese patent medicine liquid, the average pore diameter of the second porous surface is larger than that of the first porous surface, the larger pore diameter of the second porous surface is beneficial to the liquid medicine to quickly enter the sulfone polymer microporous liquid-stopping film, so that the sulfone polymer microporous liquid-stopping film has larger flux, the liquid medicine flux is ensured to be stable, the liquid medicine has higher filtration rate when passing through the sulfone polymer microporous liquid-stopping film, the filtration time of the liquid medicine can be shortened, the pore volume on unit area is large, namely the loading capacity is large, and the gaps and inter-gap fibers are small, namely the flow resistance is small; wherein the average pore diameter of the second porous surface is 7-28 μm, preferably 12-22 μm, and cannot be too large or too small, and too large pore diameter can lead to low filtration accuracy, and too small pore diameter cannot guarantee flux; particulate matters larger than 28 mu m in the liquid medicine cannot pass through the second porous surface, and prefiltering of the liquid medicine is completed, so that the filtering precision and flux stability of the microporous liquid-stopping film of the sulfone polymer disclosed by the invention are ensured, and the medication safety in practical application is ensured; meanwhile, the liquid medicine enters the microporous liquid-stopping film of the sulfone polymer from the second porous surface, and the pore volume on the unit area of the liquid inlet surface is large due to the existence of pores with the average inner diameter of 7-28 mu m, so that the liquid medicine can be uniformly and rapidly wetted on the microporous liquid-stopping film of the whole sulfone polymer, and the air in the microporous liquid-stopping film of the sulfone polymer is prevented from entering a human body; the first porous surface is used as a liquid outlet surface, wherein the average pore diameter of the first porous surface is 4-20 mu m, preferably 8-15 mu m, cannot be too large or too small, the too large pore inner diameter can lead to low filtering precision, the risk of liquid leakage exists, the too small inner diameter cannot ensure flux, and the particulate matters larger than 20 mu m in the liquid medicine cannot pass through the second porous surface to filter the liquid medicine for multiple times, so that the microporous liquid-stopping film of the sulfone polymer has higher filtering precision and stable flux, and the medication safety in practical application is ensured.

In addition, because the first porous surface is the liquid outlet surface of the liquid medicine, the liquid medicine in the whole sulfone polymer micropore liquid-stopping film and the film has bearing function, the average pore diameter of the first porous surface should not be too large, the whole strength of the sulfone polymer micropore liquid-stopping film is ensured, and the improvement is realizedThe deformation resistance of the microporous liquid-stopping film of the sulfone polymer at the liquid-stopping end point; the method for measuring the average pore diameter of the membrane surface can be used for carrying out morphology characterization on the membrane structure by using a scanning electron microscope, then carrying out measurement by using computer software (such as Matlab, NIS-Elements and the like) or manually, and carrying out corresponding calculation; in the preparation of the membrane, the characteristics such as pore size distribution are substantially uniform in the direction perpendicular to the membrane thickness (the direction is a planar direction if the membrane is in the form of a flat plate membrane; the direction is perpendicular to the radial direction if the membrane is in the form of a hollow fiber membrane); the average pore size of the whole on the corresponding plane can be reflected by the average pore size of the partial region on the plane. In practice, the surface of the film can be characterized by electron microscopy to obtain a corresponding SEM image, and a certain area, such as 1 μm, can be selected because the pores on the surface of the film are substantially uniform ² (1 μm by 1 μm) or 25 μm ² (5 μm by 5 μm), measuring the aperture of all holes on the specific area according to the actual situation, and calculating to obtain the average aperture of the surface; of course, the person skilled in the art can also obtain the above parameters by other measuring means, which are only used as reference.

Preferably, the second porous surface has a second pore density of 15-70 pores/40000 μm with a pore diameter of 10-35 μm ² ，

And the ratio of the number of the second holes with the aperture of 10-35 mu m to the number of the second holes in the whole is not less than 70%;

the first porous surface has a first pore density of 6-50 pores/40000 μm with a pore diameter of 5-25 μm ² 。

The second porous surface is used as the liquid inlet surface of the membrane, the second holes with the aperture of 10-35 mu m are more suitable holes, the holes are uniformly distributed on the second porous surface of the sulfone polymer microporous liquid-stopping film, the aperture is not too large, the too large aperture can improve the flux of the membrane, but the filtration precision of the membrane is reduced, the particulate matters easily pass through the membrane and have a certain degree of defectsPotential safety hazards, and the surface tension of the liquid medicine and the surface of the membrane is reduced, so that the capillary phenomenon is weakened, and the liquid stopping height of the membrane is influenced; the pore diameter is not too small, the flux of the membrane is reduced due to too small pore, the flow rate of the liquid medicine is influenced, the transfusion time is prolonged, and the liquid medicine of the Chinese patent medicine with higher viscosity and density is adsorbed in the membrane, so that the flux of the membrane is attenuated faster, and the use of the membrane is influenced; the second holes have a suitable pore diameter, preferably 15-30 μm, and a suitable number and ratio, preferably a pore density of 25-60 pores/40000 μm ² The method comprises the steps of carrying out a first treatment on the surface of the The ratio of the number of the holes to the number of the second holes is not less than 75%; the flux of the membrane is ensured to be large and stable enough, the flux is attenuated, the flux is still more than 90% of the initial flux after a few bottles of infusion, and the membrane is ensured to have better hydrophilicity, liquid stopping performance and higher filtering precision, so that the sulfone polymer microporous liquid stopping film has excellent comprehensive performance.

The first porous surface is used as the liquid outlet surface of the membrane, the pore diameter is preferably 8-20 μm, the pore diameter of the first porous surface is smaller than that of the second porous surface, and the pore density is preferably 10-40 pores/40000 μm ² The method comprises the steps of carrying out a first treatment on the surface of the The first porous surface has a certain supporting effect on the whole membrane, and the second porous surface has a final filtering effect on the liquid medicine, so that the filtering precision of the membrane can be further improved.

Preferably, the porous body comprises two side areas and a middle area, the middle area is a liquid stopping layer, one side area of the porous body, which is close to the second porous surface, is a pre-filtering layer, one side of the porous body, which is close to the first porous surface, is a supporting layer, and the average pore diameter of the liquid stopping layer is smaller than the average pore diameters of the pre-filtering layer and the supporting layer; the thickness of the pre-filtering layer is at least more than 15um, and the average pore diameter of the pre-filtering layer is 3-25um.

In the membrane structure of the sulfone polymer microporous liquid-stopping membrane provided by the invention, the porous main body of the sulfone polymer microporous liquid-stopping membrane comprises two side areas and a middle area in the thickness direction, wherein the liquid layer is arranged in the middle area, one side area of the porous main body, which is close to the first porous surface, is a supporting layer, one side area of the porous main body, which is close to the second porous surface, is a prefilter layer, the liquid medicine sequentially passes through the prefilter layer, the liquid-stopping layer and the supporting layer, the average pore diameter of the liquid-stopping layer is smaller than that of the prefilter layer and the supporting layer, the pores in the prefilter layer can ensure higher prefilter precision, prevent particulate matters from flowing into the liquid-stopping layer to influence the liquid-stopping effect, ensure the flux of the liquid medicine, and the pores in the supporting layer can improve the integral strength of the sulfone polymer microporous liquid-stopping membrane, and simultaneously enable the membrane to be flatter and prevent curling deformation; the holes in the liquid stopping layer can further ensure the filtering precision of the membrane, meanwhile, due to the existence of the non-directional tortuous passage of the liquid stopping layer and the small aperture of the non-directional tortuous passage of the liquid stopping layer, the friction force of the liquid medicine in the passage of the liquid stopping layer is large, and the surface tension is generated between the liquid medicine and the surface of the passage of the liquid stopping layer, so that the liquid medicine is adhered in the liquid stopping layer, and the surface tension is upward tension towards the liquid inlet surface to attract the liquid medicine below the liquid outlet surface, thereby realizing liquid stopping; if the liquid-stop layer has an excessively large pore diameter, the surface tension generated is small or no surface tension is generated, and thus liquid stop cannot be achieved.

The prefilter layer is used as the inflow side of the liquid medicine and has main prefiltering effect on the liquid medicine; in addition, the pre-filtering layer has a certain protection effect on the liquid stopping layer, because some impurities with large particle size, such as glass slag, possibly exist in the Chinese patent medicine, the glass slag is relatively sharp compared with other impurities, if the pre-filtering layer does not exist or the pre-filtering layer is too small in thickness, the glass slag is easy to contact with the liquid stopping layer in the liquid stopping film, the glass slag can scratch or even damage the liquid stopping layer, and the liquid stopping layer cannot perform a good liquid stopping effect; the thickness of the pre-filtering layer is at least larger than 15um, the average pore diameter of the pre-filtering layer is 3-25um (the thickness of the pre-filtering layer is preferably 15-35 um, the average pore diameter of the pre-filtering layer is preferably 8-20 um), and the thickness and the pore diameter of the pre-filtering layer are controlled, so that the whole flux of the membrane is ensured, the pre-filtering effect is achieved, in addition, the liquid stopping layer is protected, and the influence of relatively sharp impurities such as glass slag is avoided.

Preferably, the thickness of the microporous liquid-stopping film of the sulfone polymer is 50-150 mu m, and the average pore diameter of the PMI is 3-5 mu m; the porosity is 70-98%.

The thickness of the microporous liquid stopping film of the sulfone polymer is in the micron order, preferably 90-120 mu m, and the whole thickness of the film is thinner, so that the film is easier to be arranged in a liquid stopping device, the flow of Chinese patent medicine liquid medicine is facilitated, and the flow rate of the liquid medicine is increased; when the thickness of the microporous liquid-stopping film of the sulfone polymer is too small, the strength of the film is small; meanwhile, due to short filtering time, effective filtering cannot be performed; when the thickness of the microporous liquid-stopping film of the sulfone polymer is too large, the filtering time is too long, and the filtering efficiency is affected; therefore, when the microporous liquid-stopping film of the sulfone polymer has proper thickness, on one hand, the mechanical strength is higher, and on the other hand, the effective filtration can be carried out and the filtration efficiency is higher; the microporous liquid-stopping film of the sulfone polymer has higher porosity, preferably 85-98%, so that the microporous liquid-stopping film of the sulfone polymer is further ensured to have higher flux.

Preferably, the liquid stopping layer is of a symmetrical structure, and the pore size of one side of the liquid stopping layer close to the pre-filtering layer is basically the same as the pore size of one side of the liquid stopping layer close to the supporting layer;

the average pore diameter of the liquid stop layer is 1-13um, and the thickness is 10-40um; the average pore diameter of the supporting layer is 2-18um, and the thickness of the supporting layer is 20-60um.

Preferably, the thicknesses of the liquid-stop layer and the supporting layer are as follows: 15-30 mu m and 30-50 mu m, wherein the supporting layer is used as the outflow side of the liquid medicine, has supporting effect on the prefilter layer and the liquid stopping layer, and the thickness of the supporting layer is slightly larger than that of the prefilter layer and the liquid stopping layer so as to ensure the integral strength of the microporous liquid stopping film of the sulfone polymer and prevent the membrane from being damaged; the thinner the liquid-stopping layer, the fewer the number of holes of the liquid-stopping layer, which means that the aperture of the liquid-stopping layer is small enough to achieve the liquid-stopping effect, and as the preferred average aperture of the liquid-stopping layer and the supporting layer is: 3-10um,5-15um.

Preferably, the surface energy of the microporous liquid-stopping film of the sulfone polymer is 80-120mN/m; the initial contact angle of saturated salt water on the microporous liquid-stopping film of the sulfone polymer is 55-75 degrees, and the time for changing the contact angle to 0 degrees is 2-10s; the adhesion work is 100J/m ² -170J/m ² 。

The microporous liquid-stopping film of the sulfone polymer provided by the invention has higher hydrophilicity, high wetting speed and stronger hydrophilicity when the test liquid is saturated saline; the surface energy of the membrane is preferably 90-115mN/m; the surface energy is not limited to a certain surface of the microporous liquid-stopping film of the sulfone polymer, and can be a first porous surface or a second porous surface; by taking saturated saline as a test solution, the surface energy of the saturated saline is larger than that of water, the surface energy of the saturated saline is 81.4mN/m, and the surface energy of the water is 72.8mN/m; the hydrophilicity of the microporous liquid-stopping film of the sulfone polymer can be more accurately reflected; and one of the most common solvents used in transfusion is saline water, which is more reasonable and accurate compared with a liquid stopping film, and can further reflect the hydrophilicity of the microporous liquid stopping film of the sulfone polymer; according to the invention, the volume of a drop of saturated saline solution selected by the test solution is about 0.04-0.05ml, the area of the selected sulfone polymer microporous liquid-stopping film can at least fully absorb a drop of saturated saline solution, and the time for the drop of saturated saline solution to fully wet the sulfone polymer microporous liquid-stopping film is not more than 15s, preferably not more than 10s when the contact angle of the drop of saturated saline solution becomes 0 DEG on the first porous surface or the second porous surface of the sulfone polymer microporous liquid-stopping film; the contact angle can be accurately measured by a contact angle tester, the surface energy of the microporous liquid-stopping film of the sulfone polymer is higher, and the time for setting the contact angle edge of the saturated salt water drop on the film to be 0 DEG is short; the sulfone polymer microporous liquid-stopping film has excellent wettability, can rapidly wet saturated saline water, and can be understood that the liquid medicine can rapidly wet the film, so that residual bubbles in the film are prevented, and the liquid medicine flows into a patient during transfusion; the infusion device has higher practicability when facing emergency infusion or rescuing patients with danger.

The sulfone polymer microporous liquid-stopping film has higher circulation rate, namely higher hydrophilicity, while meeting the liquid-stopping effect, the initial contact angle of saturated salt water when the saturated salt water drops to the sulfone polymer microporous liquid-stopping film refers to the average value of the left contact angle and the right contact angle of the saturated salt water and the sulfone polymer microporous liquid-stopping film, and the shorter the contact angle becomes 0 DEG, the higher the wettability of the sulfone polymer microporous liquid-stopping film is represented. The work of adhesion is defined as an area of 1cm ² Is a solid-liquid interface of (a)The greater the work done, i.e. the more difficult the liquid will be to peel from the solid surface, the more hydrophilic the solid will be to the liquid, the more preferably the work of adhesion of saturated saline solution to the microporous liquid-stop film of sulfone polymer is 140J/m ² -170J/m ² Therefore, the saturated saline solution has stronger affinity with the membrane, and the membrane can be wetted quickly.

Preferably, the IPA complete bubble point of the microporous liquid stop film of the sulfone polymer is 9-16KPa, and the IPA initial bubble point is 6-10KPa; the ratio of the initial bubble point of the IPA to the full bubble point of the IPA is (0.55-0.85): 1.

the bubble point is an important performance characteristic of the membrane, and the application range of the liquid stopping film is greatly influenced by the height of the bubble point; bubble point testing methods are well known in the art, and the procedures for these tests are explained in detail, for example, in ASTM F316-70 and ANS/ASTM F316-70 (re-approval 1976), which are incorporated herein by reference. The test liquid used in the invention is IPA (isopropyl alcohol); the bubble point is divided into an initial bubble point and a complete bubble point; when continuous bubble emergence starts in the middle of the liquid stopping film, reading the pressure at the moment, and taking the pressure as an initial bubble point; when the membrane is fully out of bubble, the pressure at this time is read as the full out-bubble point.

Therefore, the pore diameter structure of the microporous liquid stopping film of the sulfone polymer is reflected by the initial bubble point and the complete bubble point from another angle, the maximum pore diameter in the membrane is reflected by the initial bubble point, the smaller the initial bubble point, the larger the maximum pore diameter in the membrane is, namely, a certain number (though a smaller number) of pores with larger pore diameters exist in the membrane, and the existence of the pores can further accelerate the speed of the liquid medicine to completely wet the membrane, but the weaker the capillary phenomenon generated when the liquid medicine enters the membrane is, the lower the liquid stopping height is; in addition, the existence of the large-aperture holes can lead to lower filtering precision of the membrane, large particulate matters can easily pass through, and the large particulate matters can cause harm to the body of a patient; on the contrary, the larger the initial bubble point is, the smaller the maximum aperture is, and it can be understood that all apertures in the membrane are smaller at the moment, the capillary phenomenon generated when the liquid medicine enters the membrane is strong, and the liquid stopping height is higher; however, due to the existence of the too small aperture, the membrane has a compact structure, the speed of wetting the membrane by the liquid medicine is slow, the initial liquid inlet speed and the initial liquid outlet speed of the membrane are inconsistent, the air in the membrane is slow in discharge speed or can not be completely discharged, and certain potential safety hazard exists; and the flux of the membrane is low.

The minimum aperture inside the complete bubble point reaction membrane is smaller as the complete bubble point is larger, and the proper complete bubble point of the membrane ensures that the membrane has higher interception efficiency; therefore, while ensuring the membrane wetting rate, the ratio of the IPA initial bubble point to the IPA full out bubble point of the sulfone polymer microporous liquid stopper membrane is (0.55-0.85): 1, preferably (0.6-0.8): 1, a step of; the pore diameter in the membrane is ensured to be relatively uniform, no particularly bigger pore or particularly smaller pore is existed, the pore diameter is relatively uniform, the interception efficiency of the microporous liquid-stopping film of the sulfone polymer is ensured to be high, and the complete wetting speed is fast and uniform.

Preferably, the average fiber diameter forming a porous structure in the support layer is greater than the average fiber diameter forming a porous structure in the liquid-stop layer and the prefilter layer; the average fiber diameter of the porous structure formed in the pre-filtering layer, the liquid-stopping layer and the supporting layer is sequentially 1-10 mu m,0.8-7 mu m and 2-12 mu m; the fibers in the porous main body are of strip-shaped structures; the fibrous structure can improve the overall mechanical properties of the membrane, wherein the average fiber diameter of the support layer is slightly thicker than the pre-filter layer and the liquid-stop layer, and can provide good support strength for the pre-filter layer and the liquid-stop layer.

The main body of the sulfone polymer microporous liquid-stopping film is provided with a plurality of non-directional tortuous passages, each passage is arranged along the thickness direction of the film, each passage is a flow path of liquid medicine, fibers in the main body are of a strip-shaped structure, each passage is formed by the strip-shaped fiber structure, so that the flow channel of the liquid medicine is more close to turbulence, the contact probability of the liquid medicine and the fibers is increased, the filtration efficiency is improved, the interception efficiency is ensured, and the liquid-stopping film is ensured to have higher flux; it will be appreciated that the fibrous structures are integrally interconnected, such as integrally formed, without the use of additional adhesives or the like to interconnect them, and that the network-like fibers cannot be separated from one another unless torn by an external force.

The average fiber diameter of the fibers in each region of the microporous liquid-stopping film of the sulfone polymer is different, wherein the support layer has a larger average fiber diameter and plays a strong role in supporting; the existence of the fiber with larger diameter can greatly improve the mechanical strength of the membrane, and the existence of the fiber with smaller diameter can further improve the mechanical strength of the membrane, so that the membrane has larger tensile strength and elongation at break; the larger fiber structure is favorable for intercepting the granular matters with larger particle size, the smaller fiber structure is favorable for intercepting the granular matters with smaller particle size, and finally, fine granular matters can be intercepted, so that the effective interception rate of a liquid stopping film on the granular matters can be greatly improved, and the filtering precision is high; meanwhile, due to the existence of the fiber layer with larger diameter, the flux of the liquid-stopping film is larger, the filtering time is shorter, the time cost is lower, and the economic benefit is higher; when in transfusion, a patient can adjust the liquid medicine speed according to the body condition, and the flux of the liquid stopping film is larger, so that the liquid medicine flow speed can be adjusted according to the patient to change in real time, and the time error is small.

Wherein the fibers within each layer are substantially uniformly distributed, and wherein the network-like fibers are not uniform in thickness throughout each layer, exhibit no distinct increasing or decreasing patterns, and have no distinct interfaces with abrupt changes in average fiber diameter between adjacent layers. The average fiber diameter can be calculated after the morphology of the membrane structure is characterized by using a scanning electron microscope and then the average value is measured by using computer software (such as Matlab, NIS-Elements and the like) or manually; in addition, the thickness of the whole polymer liquid-stopping film and the thickness of the three-layer structure inside the polymer liquid-stopping film can also be measured by the method; it will be appreciated that the above parameters may also be obtained by other measurement means by a person skilled in the art.

Preferably, the tensile strength of the microporous liquid-stopping film of the sulfone polymer is 3-10MPa, the elongation at break is 30-60%, and the water flux is 150-260mL min ^-1 *cm ^-2 The entrapment efficiency of the sulfone polymer microporous liquid-stopping film on impurity particles with the particle diameter not less than 5 mu m is more than 90%.

The sulfone polymer microporous liquid-stopping film has excellent mechanical properties, ensures that the film cannot be broken and fiber floccules fall off under the condition of long-time use, ensures that the film has good flux when in use, basically has consistent liquid inlet speed and liquid outlet speed, and has higher practicability; important indexes for evaluating the mechanical strength of the liquid-stopping film are the tensile strength and the elongation at break of the liquid-stopping film; under certain conditions, the greater the tensile strength of the liquid-stopping film, the better the mechanical strength of the liquid-stopping film is; tensile strength refers to the ability of a film to withstand parallel stretching; when the film sample is tested under certain conditions, the tensile load is acted until the film sample is broken, and the tensile strength and the elongation at break of the film can be calculated according to the maximum tensile load corresponding to the breaking of the film sample, the change of the size (length) of the film sample and the like; tensile strength, elongation at break, all of which can be measured by a universal tensile tester, methods of testing tensile strength are well known in the art, for example, the procedure for tensile strength testing is explained in detail in ASTM D790 or ISO 178; the tensile strength of the liquid stopping film is 3-10MPa; the elongation at break is 30-60%, which indicates that the liquid stop film of the invention has larger tensile strength and elongation at break, better mechanical property and higher industrial practical value, and can completely meet the market demand.

The permeation flux is also called as permeation rate, and is referred to as flux for short, and refers to the permeation quantity of substances passing through a unit membrane area in unit time under a certain working pressure in the separation process of a liquid membrane; the flux reflects the speed of filtration; the higher the flux, the faster the filtration rate of the membrane; the flux of the microporous liquid-stopping film of the sulfone polymer is 150-260mL min ^-1 *cm ^-2 The flux is larger, which means that the filtering speed of the liquid stopping film is higher, so that the speed of hanging drops can be adjusted, and the liquid stopping film is suitable for patients in various conditions; when the conditions allow, the infusion speed can be properly increased, and the time of a patient is saved; and the fluid can quickly pass through the liquid stopping film while the interception efficiency is ensured, the time cost is low, and the economic benefit is high.

The sulfone polymer microporous liquid-stopping film provided by the invention is prepared according to the Chinese medical industry standard YY

0770.1-2009 is tested by the requirement of the filter material for medical infusion apparatus, and the indexes such as the content of dissolved matters, the content of fluorescent matters, the falling-off amount of particles and the like all meet the standard.

The preparation method of the microporous liquid-stopping film of the sulfone polymer comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 5-20 parts of sulfone polymer, 40-75 parts of first organic solvent and 6-25 parts of hydrophilic additive;

S2: placing the liquid film in air at 10-40deg.C, and then keeping absolute humidity at 15gH ₂ O/kg-35g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.4-0.8m/s, and the duration time is 8-25s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 10-40 ℃, and the re-phase separation and solidification time is 30-150s; the coagulating bath is a mixture of a second organic solvent and water; wherein the second organic solvent is miscible with water and the first organic solvent, and the volume of the second organic solvent is 5% -25% of the volume of the mixture;

s4, performing S4; stretching the raw film by 1.05-1.5 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Preferably, the sulfone polymer comprises at least one of polyethersulfone, polysulfone, and polyarylsulfone;

the hydrophilic additive comprises polyvinyl alcohol, polyethylene glycol, polyethyleneimine and polyvinylpyrrolidone or one of the combination;

the first organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, caprolactam, N-ethyl pyrrolidone, dimethylacetamide and N-methyl pyrrolidone;

The second organic solvent is at least one of dimethyl sulfoxide, caprolactam, N-methylpyrrolidone, N-ethylpyrrolidone, dimethylformamide, dimethylacetamide, trimethyl phosphate, triethyl phosphate and r-butyrolactone.

In the method, firstly preparing a casting solution, wherein the casting solution comprises a sulfone polymer, a first organic solvent and a hydrophilic additive; the sulfone polymer is at least one of polyethersulfone, polysulfone and polyarylsulfone, and has excellent oxidation resistance, thermal stability and mechanical properties, so that the film-forming mechanical properties are excellent, various processing treatments can be satisfied, and the industrial value is high; meanwhile, the water-proof film has good hydrophilicity and is suitable for being used as a water-proof film; wherein the first organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, caprolactam, N-ethyl pyrrolidone, dimethylacetamide and N-methyl pyrrolidone, and is used for sufficiently dissolving the sulfone polymer material so as to form uniform and stable casting film liquid (homogeneous system); the hydrophilic additive is the combination of polyvinyl alcohol, polyethylene glycol, polyethyleneimine and polyvinylpyrrolidone or one of the polyvinyl alcohol, the polyethylene glycol, the polyethyleneimine and the polyvinylpyrrolidone, the viscosity of the system can be effectively controlled by adding the hydrophilic additive, macropores are prevented from being formed in the liquid film in the phase separation process, and the stability of the flux of the film can be effectively improved; in addition, the hydrophilicity of the film can be greatly improved, so that the film has higher hydrophilicity, and is suitable for being used as a liquid stopping film; by adjusting the proportions of the sulfone polymer, the first organic solvent and the hydrophilic additive, the casting solution has proper viscosity, and the viscosity of the casting solution can have a great influence on the structure and performance of the finally formed filter membrane, such as the pore diameter, thickness, flow rate and the like of the filter membrane; thereby ensuring that the finally prepared microporous liquid-stopping film of the sulfone polymer has proper thickness and ideal film pore structure and pore size;

Casting the prepared casting film on a carrier to form a liquid film; the casting solution of the present invention may be cast manually (e.g., by pouring by hand, casting, or spreading over a casting surface) or automatically (e.g., pouring or otherwise casting over a moving bed); a variety of apparatuses known in the art may be used for casting. Casting equipment includes, for example, mechanical applicators, including knives, doctor blades, or spray/plenum systems. As known in the art, a variety of casting speeds are suitable, such as casting speeds of about 2-6 feet per minute (fpm) and the like, as the case may be;

casting the self-made casting film on a carrier to form a liquid film; then the liquid film is placed at absolute humidity of 15-35g H ₂ The liquid film can be induced to conduct pre-phase separation in the O/kg wet environment; facilitating formation of coarse fibers of the support layer under such humidity conditions; in particular, the process of immersing the liquid film and the carrier together into the curing liquid is helpful for forming the structures of the layers in the liquid film and the carrier: simultaneously blowing air flow with the flow speed of 0.4-0.8m/s to the surface of the liquid film, and pre-phasing for 8-25s; thus, the liquid film can be pre-phased under the action of the wet air flow to form a first porous surface and a supporting layer, and a certain number of holes with proper pore sizes are formed on the first porous surface; the absolute humidity and the flow speed of the air flow are related to the pore size and the number of the pores on the first porous surface to a certain extent.

When the liquid film is completely immersed in the coagulating bath, the coagulating bath can not pass through one side of the carrier, and the coagulating bath can only enter the inside of the film body through the first porous surface, at the moment, the holes formed by the earlier phase separation in the supporting layer can enable the curing liquid to smoothly pass through until reaching the corresponding area before the formation of the liquid stopping layer, so that the concentration of the coagulating bath in the corresponding area before the formation of the liquid stopping layer can be quickly increased, and the area is phase-separated and cured to form the liquid stopping layer in a short time; the shorter the phase separation time, the smaller the average pore diameter, so a liquid-stopping layer with a small average pore diameter is formed; it should be emphasized that, because of the greater humidity of the air flow controlled in S2, the larger average pore size formed at the first porous surface will facilitate the rapid passage of the coagulation bath, thereby facilitating the formation of a liquid-stop layer; at the same time, the average pore size of the first porous surface and the support layer will also have a very large effect on the average pore size of the liquid-stop layer and the average pore size of the pre-filter layer and the second porous surface;

as the soaking time passes, the coagulating bath enters the corresponding area before the pre-filtering layer is formed and is further gradually diffused towards the direction of the carrier, and the concentration of the coagulating bath always has a certain gradient, namely, the concentration of the coagulating bath on the side close to the first porous surface is larger than that on the side close to the carrier, so that the concentration of the solidified liquid water in the corresponding area before the pre-filtering layer is formed is relatively lower, the phase separation time is long, and finally, the pre-filtering layer with relatively larger average pore diameter and the second porous surface with larger average pore diameter are formed;

The coagulating bath is a mixture of a second organic solvent and water, the water is a non-solvent, the second organic solvent is mutually soluble with water and is mutually soluble with the first organic solvent, the volume of the second organic solvent is 5-25% of the volume of the mixture, and the shorter the phase separation time is, the smaller the pore diameter of the formed holes is, so that the flux of the membrane is smaller; the second organic solvent with less amount can reduce the phase separation speed and prolong the phase separation time relatively, so that holes with more proper diameters are formed, the sulfone polymer microporous liquid-stopping film has enough flux, and the flux of the film decays slowly along with the prolonged drip injection time of the Chinese patent medicine.

Then air-drying to form a solid film, wherein the air-drying can be natural air-drying or air-drying by using a machine such as an electric fan; then stretching the solid film to 1.05-1.5 times of the original area; the stretching mode can form unidirectional stretching through the speed difference of the front roller and the rear roller, and can also be obtained through bidirectional stretching of the solid film; after the solid film is stretched, the mechanical strength of the film is improved, and the film becomes a tough film; and after stretching, shaping is performed, and the shaping can be heat shaping, so that the sulfone polymer microporous liquid-stopping film with an ideal film structure is obtained, has stronger hydrophilicity, can be quickly wetted by deionized water, saturated saline solution and other liquids, and further ensures the health of patients.

The application of the sulfone polymer microporous liquid stopping film in a liquid stopping device comprises a shell, the sulfone polymer microporous liquid stopping film arranged in the shell and a side cover sealed in the shell, wherein a medicine inlet and a medicine outlet are arranged in the vertical direction of the shell, the sulfone polymer microporous liquid stopping film is arranged in the shell and divides the shell into a liquid inlet cavity and a liquid outlet cavity, the medicine inlet is communicated with the liquid inlet cavity, and the medicine outlet is communicated with the liquid outlet cavity; the liquid medicine enters the liquid inlet cavity from the medicine inlet, flows to the liquid outlet cavity sequentially through the second porous surface and the first porous surface of the sulfone polymer microporous liquid-stopping film, and flows out from the medicine outlet.

The sulfone polymer microporous liquid stopping film is arranged in the liquid stopping device and is used for stopping liquid of injection liquid of plant extract liquid with higher density and viscosity, the flux of the sulfone polymer microporous liquid stopping film is larger, the infusion time is increased, the flux attenuation of the film is reduced, the condition that the flow rate of liquid medicine is slower and slower after long-time infusion of a patient is avoided, the infusion time of the patient is reduced, the flow rate of the liquid medicine can be adjusted and changed at any time by the patient according to the condition of the patient, the time delay when the flow rate of the liquid medicine is changed is reduced, and the device has higher applicability.

Preferably, the second porous surface is a liquid inlet surface and the first porous surface is a liquid outlet surface.

Compared with the prior art, the invention has the beneficial effects that: the sulfone polymer microporous liquid-stopping film provided by the technical scheme has a more optimized film body structure, and also has more optimized comprehensive performance, and has the advantages of sufficiently large and stable flux, slow flux decay, high filtering precision, excellent and stable liquid-stopping performance, larger flux and the like; the preparation method provided by the technical scheme can conveniently, quickly and effectively prepare and obtain the microporous liquid-stopping film of the sulfone polymer; according to the liquid stopper provided by the technical scheme, the liquid medicine can be filled rapidly, the flux of the liquid stopper is increased, the filtering precision of the liquid stopper is further improved, and the liquid stopper has higher applicability.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.

FIG. 1 is a Scanning Electron Microscope (SEM) image of the second porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 1 of the present invention, with magnification of 500;

FIG. 2 is a Scanning Electron Microscope (SEM) image of the first porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 1 of the present invention, wherein the magnification is 500;

FIG. 3 is a Scanning Electron Microscope (SEM) image of the second porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 3 of the present invention, with magnification of 500;

FIG. 4 is a Scanning Electron Microscope (SEM) image of the first porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 3 of the present invention, with magnification of 500;

FIG. 5 is a Scanning Electron Microscope (SEM) image of the second porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 5 of the present invention, with magnification of 500;

FIG. 6 is a Scanning Electron Microscope (SEM) image of the first porous surface of the microporous liquid stopper film of sulfone polymer prepared in example 5 of the present invention, with magnification of 500;

FIG. 7 is a schematic diagram of a device for testing bubble point of a microporous liquid-stop film of a sulfone polymer in accordance with the present invention;

FIG. 8 is a schematic diagram of a device for testing the filtration accuracy of a microporous liquid-stopping film of a sulfone polymer according to the present invention;

FIG. 9 is a schematic view of the structure of the liquid stopper according to the present invention;

Fig. 10 is a cross-sectional view of the stopper provided by the present invention.

Description of the reference numerals

1. A housing; 11. a medicine inlet; 12. a medicine outlet; 2. microporous liquid-stopping film of sulfone polymer; 3. a side cover; 4. a bracket; 5. a support rib; 51. a recess.

Detailed Description

The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

In the examples described below, the materials and equipment used to prepare the liquid stopper film are commercially available, unless otherwise specified. The method comprises the steps of preparing a liquid stopping film by using a steel belt casting machine, and characterizing the structural morphology of the liquid stopping film by using a scanning electron microscope with the model of S-5500 provided by Hitachi.

Example 1

This example 1 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 8 parts of polyethersulfone, 48 parts of dimethyl sulfoxide and 12 parts of polyvinyl alcohol;

S2: the liquid film is placed in an air environment with the temperature of 35 ℃ and then the absolute humidity is 15g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.45m/s, and the duration time is 24s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 23 ℃, and the re-phase separation and solidification time is 147s; the coagulating bath is a mixture of dimethyl sulfoxide and water; the volume of dimethyl sulfoxide was 24% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.42 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 2

This example 2 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 12 parts of polysulfone, 60 parts of dimethylformamide and 15 parts of polyethylene glycol;

s2: the liquid film was placed in an air atmosphere at 28℃and then the absolute humidity was 28g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.65m/s, and the duration time is 12s;

S3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 10 ℃, and the re-phase separation and solidification time is 72s; the coagulating bath is a mixture of dimethylformamide and water; the volume of N-methyl pyrrolidone is 9% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.5 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 3

This example 3 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 15 parts of polyarylsulfone, 62 parts of N-ethyl pyrrolidone and 24 parts of polyethylenimine;

s2: the liquid film was placed in an air atmosphere at 15℃and then the absolute humidity was 19g H ₂ The O/kg air flow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the air flow and the liquid film is 0.52m/s, and the duration time is 19s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 14 ℃, and the re-phase separation and solidification time is 127s; the coagulating bath is a mixture of N-methyl pyrrolidone and water; the volume of N-methylpyrrolidone was 17% of the volume of the mixture;

S4, performing S4; and (3) stretching the raw film by 1.21 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 4

This example 4 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 5 parts of polyethersulfone, 49 parts of dimethylacetamide and 8 parts of polyvinylpyrrolidone;

s2: the liquid film was placed in an air atmosphere at a temperature of 10℃and then the absolute humidity was 32g H ₂ The O/kg air flow is blown to the surface of the liquid film to make the liquid filmPre-phase separation, wherein the relative speed between the air flow and the liquid film is 0.71m/s, and the duration time is 10s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 28 ℃, and the re-phase separation and solidification time is 59s; the coagulating bath is a mixture of dimethylformamide and water; wherein the volume of dimethylformamide is 7% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.11 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 5

This example 5 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 17 parts of polyethersulfone, 75 parts of dimethylacetamide and 21 parts of polyvinylpyrrolidone;

s2: the liquid film was placed in an air atmosphere at a temperature of 19℃and then the absolute humidity was 35g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.8m/s, and the duration time is 8s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 39 ℃, and the re-phase separation and solidification time is 30s; the coagulating bath is a mixture of dimethylacetamide and water; wherein the volume of dimethylacetamide is 5% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.35 times of area, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 6

This example 6 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 20 parts of polyarylsulfone, 72 parts of caprolactam and 25 parts of polyethylenimine;

S2: the liquid film was placed in an air atmosphere at 40℃and then the absolute humidity was 25g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.69m/s, and the duration time is 15s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 40 ℃, and the re-phase separation and solidification time is 88s; the coagulating bath is a mixture of caprolactam and water; wherein the volume of caprolactam is 11% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.27 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 7

This example 7 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 10 parts of polysulfone, 52 parts of N-ethyl pyrrolidone and 13 parts of polyethylene glycol;

s2: the liquid film was placed in an air atmosphere at 24℃and then the absolute humidity was 17g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.41m/s, and the duration time is 22s;

S3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 35 ℃, and the re-phase separation and solidification time is 132s; the coagulating bath is a mixture of N-methyl pyrrolidone and water; wherein the volume of N-methylpyrrolidone is 21% of the volume of the mixture;

s4, performing S4; and (3) stretching the raw film by 1.09 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Example 8

This example 8 provides a microporous liquid stopper film of sulfone polymer prepared by the following method: the method comprises the following steps:

s1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 13 parts of polyarylsulfone, 58 parts of dimethyl sulfoxide and 18 parts of polyvinylpyrrolidone;

s2: the liquid film was placed in an air atmosphere at a temperature of 32℃and then the absolute humidity was 21g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.58m/s, and the duration time is 17s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 17 ℃, and the re-phase separation and solidification time is 101s; the coagulating bath is a mixture of r-butyrolactone and water; wherein the volume of r-butyrolactone is 15% of the volume of the mixture;

S4, performing S4; and (3) stretching the raw film by 1.3 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

Comparative example one

Any common liquid stopping film in the market is selected, and the film is tested by a PMI aperture tester, wherein the number of holes with the PMI aperture of not more than 2.5 mu m accounts for 43% of the total number of holes, and the number of holes with the PMI aperture of more than 6 mu m accounts for 10% of the total number of holes.

Comparative example two

Any common liquid stopping film in the market is selected, and the film is tested by a PMI aperture tester, wherein the number of holes with the PMI aperture of not more than 2.5 mu m accounts for 5% of the total number of holes, and the number of holes with the PMI aperture of more than 6 mu m accounts for 39% of the total number of holes.

1. Structural characterization

The performance characteristics of the above examples and selected comparative examples are shown in Table 1

TABLE 1

The thickness and porosity of the sulfone polymer microporous liquid-stop film, the thickness of each layer, the average pore diameter and the average fiber diameter were measured by scanning electron microscopy on the morphological characteristics of the longitudinal sections of the sulfone polymer microporous liquid-stop film obtained in each example and comparative example, respectively, and are shown in Table 2.

TABLE 2

2. Flux testing

The same specifications (1 x 1 cm) as those of the comparative examples were selected from the above examples ² ) A microporous liquid-stopping film of a sulfone polymer; the flux of the plant extraction injection, western medicine injection and water passing through the membrane is measured, and the specific test method comprises the following steps: under other identical conditions, the initial flux of the membrane is measured by a certain volume of water, then the same volume of test liquid is passed through the membrane, and then the final flux is measured by the water passing through the membrane; the test solutions are respectively as follows: respectively 50mL of oldenlandia diffusa liquid medicine, 50mL of oldenlandia diffusa liquid medicine after 5 times dilution, 50mL of xiangdan injection after 5 times dilution, 50mL of glucose solution and 50mL of water.

The membrane flux was calculated as follows:

the calculation formula of the membrane flux (J) is as follows: j=v/(t×a) formula:

j-membrane flux unit: mL/min ^-1 /cm ^-2 The method comprises the steps of carrying out a first treatment on the surface of the V- -sample volume (ml); t- -sampling time (min); a- -effective area of membrane (cm) ² )

TABLE 3 Table 3

3. Performance testing

And (3) testing the filtering precision: the filtration membranes obtained in each example were tested for interception efficiency.

Experimental facilities: tianjin root particle counter KB-3; experiment preparation: the experimental device was assembled according to fig. 9, ensuring the device was clean, and rinsed with ultrapure water; a sample with a diameter of 47mm is taken and placed in the butterfly filter, so that the air tightness of the assembled filter is ensured to be good.

The experimental steps are as follows: pouring the challenge liquid into a storage tank, paying attention to the exhaust of a butterfly filter, pressurizing to 10kPa, and taking out the butterfly downstream filtrate by using a clean bottle; the number of particles in the filtrate and stock solutions was measured with a particle counter.

Interception efficiency:

/>

wherein: η -interception efficiency,%; n 0-number of particles in stock solution, average of 5 counts, one; n 1-number of particles in filtrate, average of 5 counts.

Through interception efficiency test: the filtration precision of the microporous liquid-stopping film of the sulfone polymer prepared in the examples 1 to 8 for impurity particles of 5 μm is more than 95%; the filtration accuracy of the liquid stopper film of comparative example 1 was 98% for impurity particles of 5 μm; the liquid stopper film of comparative example 2 had a filtration accuracy of 72% for impurity particles of 5. Mu.m.

Bubble point test

The initial bubble point of water and the complete bubble point of water for the test sample (test apparatus as shown in FIG. 8)

The experimental steps are as follows:

step one: closing the air pressure regulator, opening the air pressure regulator to enable the pressure to be higher than the tested pressure, taking out the wetted microporous liquid stopping film of the sulfone polymer to be tested, and installing the microporous liquid stopping film on a filtering device.

Step two: the reservoir was filled with 80% of the test liquid, the air pressure was increased, and the pressurization was stopped when the reservoir reached about 80% of the bubble point. It was confirmed that the sulfone polymer microporous liquid-stopper film in the reservoir had not yet been foamed at this time.

Step three: slowly boosting, and when continuous bubble emergence is started in the middle of the microporous liquid stop film of the sulfone polymer, reading the pressure at the moment as an initial bubble point. Continuing to boost, when all the microporous liquid stopping film of the sulfone polymer is foamed, reading the pressure at the moment as the maximum bubble point

Note that: typically, bubbles emerge near the center of the microporous liquid stopper film of sulfone polymer.

TABLE 4 Table 4

As can be seen from the table, the microporous liquid stopping film of the sulfone polymer prepared by the invention has larger flux and complete bubble point, and is suitable for the field of liquid stopping medical treatment.

The invention also provides application of the sulfone polymer microporous liquid-stopping film in a liquid stopper, the liquid stopper comprises a shell 1, a sulfone polymer microporous liquid-stopping film 2 arranged in the shell 1 and a side cover 3 sealed in the shell 1, a medicine inlet 11 and a medicine outlet 12 are arranged in the vertical direction of the shell 1, the sulfone polymer microporous liquid-stopping film 2 is arranged in the shell 1 and divides the shell 1 into a liquid inlet cavity and a liquid outlet cavity, the medicine inlet 11 is communicated with the liquid inlet cavity, and the medicine outlet 12 is communicated with the liquid outlet cavity; the liquid medicine enters the liquid inlet cavity from the medicine inlet 11, flows to the liquid outlet cavity sequentially through the second outer surface and the first outer surface of the sulfone polymer microporous liquid-stopping film 2, and flows out from the medicine outlet 12.

Specifically, the inside of the shell 1 is provided with a bracket 4 forming a seal with the inner wall of the shell, the bracket 4 forms a first mounting surface towards one side of the side cover 3, the middle of the bracket 4 is provided with an opening, the opening extends from the first mounting surface and penetrates through the whole thickness of the bracket 4, the edge of the sulfone polymer microporous liquid-stopping film 2 is fixed on the first mounting surface in a sealing way, and the second outer surface of the sulfone polymer microporous liquid-stopping film 2 is arranged towards the side cover 3 and forms a liquid inlet cavity with the side cover 3 and the side wall of the shell 1; the first outer surface of the sulfone polymer microporous liquid-stopping film 2 and the opening of the bracket 4 form a liquid outlet cavity with the side wall of the shell 1; the inner wall of the liquid outlet cavity is provided with supporting ribs 5, the first outer surface of the sulfone polymer microporous liquid-stopping film 2 and the supporting ribs 5 are arranged at intervals, and the supporting ribs 5 can prevent the sulfone polymer microporous liquid-stopping film 2 from deforming; the support rib 5 is provided with a plurality of concave parts 51 towards one side of the sulfone polymer micropore liquid stopping film 2, the concave parts 51 can be provided with a plurality of concave parts 51, the concave parts 51 are arranged at intervals, the space of a liquid outlet cavity of the liquid stopper can be enlarged by the concave parts 51, the liquid medicine in the liquid outlet cavity can flow out conveniently, and the liquid medicine flow speed is accelerated.

Or, the liquid stopper can be formed by at least two sulfone polymer micropore liquid stopping films 2, the sulfone polymer micropore liquid stopping films 2 are vertically arranged in the shell 1 at intervals, the shell 1 is sequentially divided into a first liquid inlet cavity, a liquid outlet cavity and a second liquid inlet cavity, liquid medicine can enter the first liquid inlet cavity and/or the second liquid inlet cavity at the same time, the flux of the liquid stopper is increased, and the arrangement of the sulfone polymer micropore liquid stopping films 2 further improves the filtering precision of the liquid stopper and has more applicability.

The liquid stopper is internally provided with the sulfone polymer micropore liquid-stopping film 2, the wetting speed of the sulfone polymer micropore liquid-stopping film 2 is high, when the liquid stopper is used, liquid medicine can be filled in the liquid stopper rapidly, gas in the membrane or in front of the membrane in the liquid stopper is prevented from entering a human body in the process of transfusion, harm to human health, such as air embolism and the like, and simultaneously, the panic of a patient is avoided, and psychological pressure of the patient can be relieved; secondly, because the liquid stopper can be filled with liquid medicine rapidly, it can be understood that the existence of the liquid stopper can not influence the flow rate of the liquid medicine, and a patient can adjust and change the flow rate of the liquid medicine at any time according to the situation of the patient, so that the time delay of the change of the flow rate of the liquid medicine is reduced, and the liquid medicine has higher applicability.

The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.

Claims (11)

1. A sulfone polymer microporous liquid-stopping film comprising a first porous surface, a second porous surface, and a porous body between the first porous surface and the second porous surface, the porous body having a non-directional tortuous path therein, characterized in that the sulfone polymer microporous liquid-stopping film is used for stopping an injection liquid comprising a botanical extract;

In the sulfone polymer microporous liquid-stopping film, the ratio of the number of holes with the aperture not exceeding 2.5 mu m measured by a PMI aperture tester to the whole number of holes is less than 10% and more than or equal to 2%;

the porosity of the microporous liquid-stopping film of the sulfone polymer is at least 60%;

the water BP value of the microporous liquid stopping film of the sulfone polymer is 20-50kPa, and the liquid stopping height is at least 1m;

in the sulfone polymer microporous liquid-stopping film, the ratio of the number of holes with the aperture exceeding 6 mu m measured by a PMI aperture tester to the total number of holes is 1-12%;

the first porous surface is provided with a plurality of first holes, and the average pore diameter of the first holes is 4-20 mu m;

the second porous surface is provided with a plurality of second holes, and the average pore diameter of the second holes is 7-28 mu m;

the porous main body comprises two side areas and a middle area, the liquid layer is arranged in the middle area, a pre-filtering layer is arranged in the area, close to the second porous surface, of the porous main body, a supporting layer is arranged in the area, close to the first porous surface, of the porous main body, and the average pore diameter of the liquid layer is smaller than that of the pre-filtering layer and the supporting layer; the thickness of the pre-filtering layer is at least larger than 15 mu m, and the average pore diameter of the pre-filtering layer is 3-25 mu m;

The average pore diameter of the liquid stop layer is 1-13 mu m, and the thickness is 10-40 mu m; the average pore diameter of the supporting layer is 2-18 mu m, and the thickness of the supporting layer is 20-60 mu m.

2. The sulfone polymer microporous liquid-stop film according to claim 1, wherein the second porous surface has a pore density of 15-70 pores/40000 μm of second pores with a pore diameter of 10-35 μm ² ，

And the ratio of the number of the second holes with the aperture of 10-35 mu m to the number of the second holes in the whole is not less than 70%;

the first porous surface has a first pore density of 6-50 pores/40000 μm with a pore diameter of 5-25 μm ² 。

3. The microporous liquid-stopping film of sulfone polymer according to claim 1, characterized in that the thickness of said microporous liquid-stopping film of sulfone polymer is 50-150 μm, and the PMI average pore diameter is 3-5 μm; the porosity is 70-98%.

4. The microporous liquid-stopping film of sulfone polymer according to claim 1, wherein said liquid-stopping layer has a symmetrical structure, and the pore size of the side of said liquid-stopping layer near the prefilter layer is substantially the same as the pore size of the side of said liquid-stopping layer near the support layer.

5. The sulfone polymer microporous liquid-stop film according to claim 1, characterized in that the surface energy of the sulfone polymer microporous liquid-stop film is 80-120mN/m; the initial contact angle of saturated salt water on the microporous liquid-stopping film of the sulfone polymer is 55-75 degrees, and the time for changing the contact angle to 0 degrees is 2-10s; the adhesion work is 100J/m ² -170J/m ² 。

6. The microporous liquid stopper membrane of sulfone polymer according to claim 1, characterized in that the IPA complete bubble point of the microporous liquid stopper membrane of sulfone polymer is 9-16kPa, and the IPA initial bubble point is 6-10kPa; the ratio of the initial bubble point of the IPA to the full bubble point of the IPA is (0.55-0.85): 1.

7. the sulfone polymer microporous liquid-stop film according to claim 1, characterized in that the average fiber diameter forming a porous structure in the support layer is larger than the average fiber diameters forming a porous structure in the liquid-stop layer and the prefilter layer; the average fiber diameter of the porous structure formed in the pre-filtering layer, the liquid-stopping layer and the supporting layer is sequentially 1-10 mu m,0.8-7 mu m and 2-12 mu m; the fibers in the porous main body are all in a strip-shaped structure.

8. The sulfone polymer microporous liquid-stop film according to claim 1, wherein the sulfone polymer microporous liquid-stop film has a tensile strength of 3-10MPa, an elongation at break of 30-60%, and a water flux of 150-260ml x min ^-1 *cm ^-2 The entrapment efficiency of the sulfone polymer microporous liquid-stopping film on impurity particles with the particle diameter not less than 5 mu m is more than 90%.

9. The method for preparing a microporous liquid stopper film of a sulfone polymer as set forth in any one of claims 1 to 8, comprising the steps of:

S1: preparing a casting film liquid, and casting the casting film liquid on a carrier to form a liquid film; the casting film liquid comprises the following substances in parts by weight: 5-20 parts of sulfone polymer, 40-75 parts of first organic solvent and 6-25 parts of hydrophilic additive;

s2: placing the liquid film in air at 10-40deg.C, and then keeping absolute humidity at 15g H ₂ O/kg-35g H ₂ The O/kg airflow is blown to the surface of the liquid film, so that the liquid film is pre-split, the relative speed between the airflow and the liquid film is 0.4-0.8m/s, and the duration time is 8-25s;

s3: immersing the liquid film after pre-phase separation into a coagulating bath for re-phase separation and solidification to form a green film, wherein the coagulating bath temperature is 10-40 ℃, and the re-phase separation and solidification time is 30-150s; the coagulating bath is a mixture of a second organic solvent and water; wherein the second organic solvent is miscible with water and the first organic solvent, and the volume of the second organic solvent is 5% -25% of the volume of the mixture

S4, performing S4; stretching the raw film by 1.05-1.5 times, cleaning in pure water, and finally drying to obtain the microporous liquid-stopping film of the sulfone polymer.

10. The method for producing a microporous liquid stopper film of a sulfone polymer according to claim 9, wherein the sulfone polymer comprises at least one of polyethersulfone, polysulfone, and polyarylsulfone;

The hydrophilic additive comprises polyvinyl alcohol, polyethylene glycol, polyethyleneimine and polyvinylpyrrolidone or one of the combination;

the first organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, caprolactam, N-ethyl pyrrolidone, dimethylacetamide and N-methyl pyrrolidone;

the second organic solvent is at least one of dimethyl sulfoxide, caprolactam, N-methylpyrrolidone, N-ethylpyrrolidone, dimethylformamide, dimethylacetamide, trimethyl phosphate, triethyl phosphate and r-butyrolactone.

11. Use of a sulfone polymer microporous liquid-stopping film according to any one of claims 1-8 in a liquid-stopping device, wherein the liquid-stopping device comprises a shell, the sulfone polymer microporous liquid-stopping film arranged in the shell and a side cover sealed to the shell, a medicine inlet and a medicine outlet are arranged in the vertical direction of the shell, the sulfone polymer microporous liquid-stopping film is arranged in the shell, the shell is divided into a liquid inlet cavity and a liquid outlet cavity, the medicine inlet is communicated with the liquid inlet cavity, and the medicine outlet is communicated with the liquid outlet cavity; the liquid medicine enters the liquid inlet cavity from the medicine inlet, flows to the liquid outlet cavity sequentially through the second porous surface and the first porous surface of the sulfone polymer microporous liquid-stopping film, and flows out from the medicine outlet.

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