CN109180985B - SiO utilizing micron-sized hollow mesoporous2Microsphere and PDMS (polydimethylsiloxane) blending crosslinking modified anti-freezing medical silica gel material - Google Patents
SiO utilizing micron-sized hollow mesoporous2Microsphere and PDMS (polydimethylsiloxane) blending crosslinking modified anti-freezing medical silica gel material Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
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- C08K7/26—Silicon- containing compounds
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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Abstract
The invention discloses a method for preparing SiO by using micron-sized hollow mesoporous SiO2The anticoagulant medical silica gel material modified by blending and crosslinking microspheres and PDMS adopts novel micron-sized reaction type hollow mesoporous SiO2The microspheres are used as a cross-linking agent and are blended with the existing silicone rubber base material for the breathing machine pipeline, namely Polydimethylsiloxane (PDMS), so that the porous microsphere doped silicone rubber base material with stable performance is obtained. Mesoporous hollow SiO2The microspheres not only can play a role in heat preservation and heat insulation, but also can load a small-molecule bacteriostatic agent therein, and the mesoporous shell layer of the microspheres enables the bacteriostatic agent to be slowly released in the base material to play a role in pipeline bacteriostasis. Finally, fixing a layer of nano SiO on the surface of the silica gel in situ2The particle super-hydrophilic layer inhibits water drops from generating on the surface, thereby preparing the novel medical silicon rubber material integrating heat preservation and insulation, anticoagulation water and bacteriostasis functions.
Description
Technical Field
The invention belongs to the technical field of medical materials, and particularly relates to a method for preparing a hollow mesoporous SiO film by using micron-sized hollow mesopores2Microsphere and PDMS are blended, cross-linked and modified to obtain the anticoagulant silica gel material.
Background
Severe medicine is rapidly developing and mechanical ventilation plays an important role in the rescue of severe patients. However, in the process of mechanical ventilation by using a ventilator, a large amount of condensed water (800-. Condensed water directly enters a pipeline or a respiratory tract to cause the water accumulation of the pipeline to be unsmooth, the respirator is triggered by mistake, man-machine confrontation is increased, further the respiratory load of a patient is increased, and the patient can be endangered by airway injury, pneumothorax, unsmooth airway and the like in serious cases.
At present, heating wires are mostly placed in an air supply pipeline to reduce the generation of condensed water, and a water collecting cup is placed in a breathing loop to promote the drainage of the condensed water and the like to reduce the medical risk caused by excessive condensed water. However, the above methods all have disadvantages, such as difficulty in achieving accurate temperature control, no heating guide wire in the exhaust pipeline, and frequent occurrence of the condition that the water collecting cup is inclined or inverted obviously when the critical patient is in position replacement and nursing operation. Condensed water in the breathing machine pipeline and the water collecting cup is also an important place for bacterial reproduction, according to statistics, the positive rate of bacterial culture reaches up to 86.7 percent, and the bacteria cultured by the sputum and the bacteria cultured in the condensed water are found to have high consistency. The concentration of bacteria in the condensate near the conduit may be as high as 2 x 105cfu/ml, increases the incidence of ventilator-associated pneumonia, and brings great difficulty to medical treatment prevention and control. The situations can lead to a series of problems of prolonged hospitalization time of ICU patients, increased treatment cost, increased medical care workload and the like, and heavy burden is brought to families and society of the patients, so that the problem of preventing condensed water in a pipeline loop of a breathing machine is one of difficult problems which are difficult to avoid clinically and urgently need to be solved by ICU.
At present, the two main flow modes of reducing the pipeline condensed water by modifying the water collecting cup or putting the pipeline heating guide wire have little effect in clinical practice, and the problems that the prior silica gel pipeline material has poor heat insulation effect, so that the inside and the outside of the pipeline can quickly exchange heat, the moisture in the hot gas in the pipeline is quickly condensed, and a large amount of condensed water is generated cannot be fundamentally solved. For the reasons, the silicon rubber material of the existing breathing machine loop is expected to be researched, the physical structure of the base material is changed or the base material is modified to improve the heat preservation and heat insulation performance of the tube, or a super-hydrophilic anti-fog coating is coated on the surface of the material to inhibit the condensation of water vapor on the surface, so that the formation of the condensed water of the breathing pipeline is completely avoided. On the other hand, the pipeline is provided with the antibacterial coating, which can play a certain role in sterilizing condensed water and excrement in the pipeline and reduce the incidence rate of hospital infection. Therefore, if the preparation and performance improvement of the anti-condensation silica gel material are successfully applied to the preparation of the silica gel material for the medical breathing pipeline, the condensation amount of the medical breathing pipeline is reduced to a great extent, the possibility of iatrogenic accidents of patients is reduced, VAP is prevented, bacterial drug resistance is reduced, the medical care working efficiency is greatly improved, and social resources are saved.
The practical function improvement of the widely popularized breathing machine pipeline material is provided from the practical problem of ICU clinical, so that the clinical practical problem is solved, and a new idea and a new method are provided for developing medical intelligent safety silica gel materials.
Disclosure of Invention
The invention aims at solving the technical problem of providing a method for utilizing micron-sized hollow mesoporous SiO2Microsphere and PDMS are blended, cross-linked and modified to obtain the anticoagulant silica gel material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
SiO utilizing micron-sized hollow mesoporous2The microsphere and PDMS blended crosslinking modified anticoagulant silica gel material for medical use is characterized in that the preparation method comprises the following steps:
(1) micron-sized hollow mesoporous SiO2Synthesizing microspheres:
i) preparing polystyrene microspheres by adopting a soap-free emulsion method, wherein an initiator adopts water-soluble potassium persulfate, and the initiator and the potassium persulfate react for 24 hours at the temperature of 70 ℃ under the protection of nitrogen to obtain monodisperse micron-sized polystyrene template microspheres;
ii) dispersing the polystyrene template microspheres obtained in the step i) in an ethanol water solution containing a trace amount of tetraethyl orthosilicate, dropwise adding a proper amount of ammonia water, reacting at room temperature for 24 hours, and performing hydroxyl modification on the surfaces of the polystyrene template microspheres;
iii) adding sixteen kinds of additives into the reaction system in the step ii)Alkyl trimethyl ammonium bromide, cyclohexane and tetraethyl orthosilicate are reacted for a period of time at 50-55 ℃ to obtain hollow mesoporous SiO2Microspheres;
iiii) forming hollow mesoporous SiO2The microspheres are dispersed in benzalkonium bromide solution and are hollow mesoporous SiO2The microspheres are loaded with small molecular bacteriostatic agents;
(2) micron-sized hollow mesoporous SiO2And (3) synthesis of microsphere crosslinked silica gel:
preparing the hollow mesoporous SiO with a large number of hydroxyl groups on the surface prepared in the step (1)2Mixing the microspheres and polydimethylsiloxane, and adding a catalyst stannous octoate to prepare silicon rubber;
(3) nano SiO on silicon rubber surface2Modifying the super-hydrophilic coating of the particles:
solid SiO with about 50nm is prepared by sol-gel method2The nano particles are dispersed in a TEOS ethanol solution, a layer of nano particles is uniformly coated on the surface of the silicon rubber by adopting a spin-coating method or a soaking and pulling method, a small amount of ammonia water is dripped to enable the nano particles to be crosslinked, and the particle layer is fixed on the surface of the silicon rubber.
The invention has the beneficial effects that:
1. the invention researches the silicon rubber material of the prior breathing circuit, changes the physical structure of the base material or modifies the base material to improve the heat preservation and heat insulation performance of the tube, thereby fundamentally solving the problem of breathing circuit condensate water during mechanical ventilation.
2. The new material breathing machine pipeline need not to install the cup device that catchments, practices thrift manufacturing cost, simplifies the pipeline installation, reduces work load.
3. Using hollow mesoporous SiO2The microspheres replace a common micromolecular silica gel cross-linking agent, and the porous heat-insulating material is ingeniously and stably introduced into the silica gel base material, so that the heat-insulating function of the material is realized, the gas temperature loss of a breathing loop is prevented, and the formation of pipeline condensed water is obviously reduced.
4. Through to material surface modification, make thermal-insulated silica gel material form super hydrophilic surface, improve the surface and prevent atomizing performance, further make steam can't condense on silica gel pipe wall surface, the pipeline is difficult to form rivers, has avoided the false triggering of breathing machine, and the at utmost reduces the man-machine to the resistance, provides accurate respiratory mechanics monitoring index, provides respiratory support for severe respiratory failure.
6. The material is loaded with and slowly releases the bacteriostat, thereby realizing the double functions of heat insulation and bacteriostasis, preliminarily disinfecting the secretion in the exhalation pipeline and the pipeline condensed water, reducing pollution and playing an important role in hospital control.
7. The new material pipeline is different from the existing disposable breathing pipeline material, is not easy to damage and differentiate, has constant performance, can endure repeated washing, disinfection and drying treatment of a disinfection supply center, meets the requirement of recycling, reduces the medical cost and saves a large amount of social resources.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of a process for preparing a silica gel material according to the present invention.
FIG. 2 shows the hollow mesoporous SiO of the present invention2Schematic diagram of microsphere synthesis principle.
FIG. 3 shows that the bacteriostatic agent of the invention is in hollow mesoporous SiO2Schematic diagram of loading in microspheres.
FIG. 4 shows the hollow mesoporous SiO of the present invention2Schematic diagram of the principle of blending and crosslinking microspheres and PMDS.
FIG. 5 shows the surface of the silicone rubber of the present invention with nano SiO2Schematic diagram of modification principle of super-hydrophilic coating of particles.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
As shown in fig. 1 to 5, a method for preparing SiO with micro-sized hollow mesopores2The preparation method of the anticoagulant silica gel material with microspheres and PDMS blended, crosslinked and modified comprises the following steps:
(1) micron-sized hollow mesoporous SiO2Synthesizing microspheres:
i) preparing polystyrene microspheres by adopting a soap-free emulsion method, wherein an initiator adopts water-soluble potassium persulfate, and the initiator and the potassium persulfate react for 24 hours at the temperature of 70 ℃ under the protection of nitrogen to obtain monodisperse micron-sized polystyrene template microspheres;
ii) dispersing the polystyrene template microspheres obtained in the step i) in an ethanol water solution containing a trace amount of tetraethyl orthosilicate, dropwise adding a proper amount of ammonia water, reacting at room temperature for 24 hours, and performing hydroxyl modification on the surfaces of the polystyrene template microspheres;
iii) adding hexadecyl trimethyl ammonium bromide, cyclohexane and tetraethyl orthosilicate into the reaction system in the step ii), and reacting for a period of time at 50-55 ℃ to obtain the hollow mesoporous SiO2Microspheres;
iiii) forming hollow mesoporous SiO2The microspheres are dispersed in benzalkonium bromide solution and are hollow mesoporous SiO2The microspheres are loaded with small molecular bacteriostatic agents;
(2) micron-sized hollow mesoporous SiO2And (3) synthesis of microsphere crosslinked silica gel:
preparing the hollow mesoporous SiO with a large number of hydroxyl groups on the surface prepared in the step (1)2Mixing the microspheres and polydimethylsiloxane, and adding a catalyst stannous octoate to prepare silicon rubber;
(3) nano SiO on silicon rubber surface2Modifying the super-hydrophilic coating of the particles:
solid SiO with about 50nm is prepared by sol-gel method2The nano particles are dispersed in a TEOS ethanol solution, a layer of nano particles is uniformly coated on the surface of the silicon rubber by adopting a spin-coating method or a soaking and pulling method, a small amount of ammonia water is dripped to enable the nano particles to be crosslinked, and the particle layer is fixed on the surface of the silicon rubber.
The invention discloses a research on condensation water resistance of a silicone rubber material, which comprises the following steps:
after the silicon rubber is crosslinked in the tubular mold, the silicon rubber is taken out and arranged on a simulated breathing pipeline for carrying out:
a. two sections of the prepared cross-linked silicone rubber tube (experimental group) which are 25cm in total are taken as an inspiratory tube and are connected by a Y-shaped connecting tube, a water collecting cup A1 is arranged below the Y-shaped tube, a thermometer 1 and a thermometer 2 are respectively arranged at the beginning and the tail end of the tube, a water collecting cup B1 is arranged in the expiratory tube by the same method, and a respirator, a 810 humidification pot and an artificial simulated lung are sequentially connected.
b. Taking two sections of silica gel threaded pipes (control group) of a traditional breathing machine pipeline, which are 25cm in total, as an inhalation pipeline, connecting the two sections by using a Y-shaped connecting pipe, installing a water collecting cup A2 below the Y-shaped pipe, respectively installing a thermometer 3 and a thermometer 4 at the beginning and the tail end of the pipeline, installing a water collecting cup B2 in the exhalation pipeline by the same method, and sequentially connecting a breathing machine, a 810 humidification tank and an artificial simulated lung.
c. The mechanical aeration was carried out for 24 hours, and the amounts of condensed water A1, B1, A2 and B2 were collected every 2 hours, and data were recorded, and the amounts of condensed water A1+ B1 and A2+ B2 were compared, and statistical analysis was performed as shown in Table 1 below.
TABLE 1
d. According to the table analysis result, the condensate water resistance of the pipeline made of the material is obviously superior to that of the traditional silica gel material.
The research on the heat preservation performance of the silicone rubber material comprises the following steps:
a. two sections of the prepared cross-linked silicone rubber tube (experimental group) which are 25cm in total are taken as an inspiratory tube and are connected by a Y-shaped connecting tube, a water collecting cup A1 is arranged below the Y-shaped tube, a thermometer 1 and a thermometer 2 are respectively arranged at the beginning and the tail end of the tube, a water collecting cup B1 is arranged in the expiratory tube by the same method and is connected with a breathing machine, a humidification pot 810 and an artificial simulated lung.
b. Taking two sections of silica gel threaded pipes (control group) of a traditional breathing machine pipeline, which are 25cm in total, as an inhalation pipeline, connecting the two sections by using a Y-shaped connecting pipe, installing a water collecting cup A2 below the Y-shaped pipe, installing a thermometer 3 and a thermometer 4 at the beginning and the tail end of the pipeline respectively, installing a water collecting cup B2 in the exhalation pipeline by the same method, and connecting a breathing machine, a 810 humidification tank and an artificial simulated lung.
c. Mechanical aeration was carried out for 24 hours, and the cold temperatures of thermometer 1, thermometer 2, thermometer 3, thermometer 4 and room temperature T0 were recorded every 2 hours, comparing the temperature differences of thermometer 1 and thermometer 2, thermometer 1 and thermometer 3, and thermometer 3 and thermometer 4, respectively, and the statistical table is shown in table 2 below.
TABLE 2
d. According to the analysis result in table 2, the heat insulation performance of the material pipeline is obviously superior to that of the existing traditional silicon rubber material.
The research on the antibacterial performance of the silicone rubber material comprises the following steps:
a. taking two sections of the prepared cross-linked silicone rubber tube (experimental group) which are 25cm in total as an inhalation pipeline, connecting the two sections of the prepared cross-linked silicone rubber tube by using a Y-shaped connecting tube, installing a water collecting cup A1 below the Y-shaped tube, installing a thermometer 1 and a thermometer 2 at the beginning and the tail end of the pipeline respectively, selecting the cross-linked silicone rubber tube containing the prepared exhalation pipeline, inoculating streptococcus pneumoniae and staphylococcus epidermidis at the near end of simulated lung exhalation respectively, installing a water collecting cup B1 in the exhalation pipeline by the same method, and connecting a breathing machine, a 810 humidification tank and an artificial simulated lung.
b. Taking two sections of silica gel threaded pipes (control group) of a traditional breathing machine pipeline, which are 25cm in total, as an inhalation pipeline, connecting the two sections by using a Y-shaped connecting pipe, installing a water collecting cup A2 below the Y-shaped pipe, respectively installing a thermometer 3 and a thermometer 4 at the beginning and the tail end of the pipeline, installing a water collecting cup B2 in the exhalation pipeline (without an antibacterial coating) in the same way, and connecting the breathing machine, a 810 humidification tank and an artificial simulated lung.
c. Mechanical aeration was carried out for 168 hours, and the end of the ventilator circuit and the catchments B1 and B2 were directly smeared with cotton swabs soaked with sterile eluant containing the corresponding neutralizing agent at 48h, 72h, 168h, respectively. The sampling tube is shaken for 20s on a blending machine, 1.0ml of sample to be detected is absorbed by a sterile suction tube and inoculated on a sterilized plate, and the sterilized plate is placed in an incubator at (36 +/-1) DEG C for culturing for 48 h. The growth of bacteria at different sites, colony counts and time dependence were compared. And in the sampling process, the hand hygiene standard and strict aseptic operation are performed. The statistical results are shown in table 3 below.
TABLE 3
According to the analysis result, the bacteriostatic performance of the pipelines of the two materials is compared, and the bacteriostatic effect of the silicon rubber material added into the gaps of the bacteriostatic agent is obviously superior to that of the traditional breathing pipeline.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the spirit of the invention or exceeding the scope defined by the claims.
Claims (1)
1. SiO utilizing micron-sized hollow mesoporous2The microsphere and PDMS blended crosslinking modified anticoagulant silica gel material for medical use is characterized in that the preparation method comprises the following steps:
(1) micron-sized hollow mesoporous SiO2Synthesizing microspheres:
i) preparing polystyrene microspheres by adopting a soap-free emulsion method, wherein an initiator adopts water-soluble potassium persulfate, and the initiator and the potassium persulfate react for 24 hours at the temperature of 70 ℃ under the protection of nitrogen to obtain monodisperse micron-sized polystyrene template microspheres;
ii) dispersing the polystyrene template microspheres obtained in the step i) in an ethanol water solution containing a trace amount of tetraethyl orthosilicate, dropwise adding a proper amount of ammonia water, reacting at room temperature for 24 hours, and performing hydroxyl modification on the surfaces of the polystyrene template microspheres;
iii) adding hexadecyl trimethyl ammonium bromide, cyclohexane and tetraethyl orthosilicate into the reaction system in the step ii), and reacting for a period of time at 50-55 ℃ to obtain the hollow mesoporous SiO2Microspheres;
iiii) forming hollow mesoporous SiO2The microspheres are dispersed in benzalkonium bromide solution and are hollow mesoporous SiO2The microspheres are loaded with small molecular bacteriostatic agents;
(2) micron-sized hollow mesoporous SiO2And (3) synthesis of microsphere crosslinked silica gel:
preparing the hollow mesoporous SiO with a large number of hydroxyl groups on the surface prepared in the step (1)2Mixing the microspheres and polydimethylsiloxane, and adding a catalyst stannous octoate to prepare silicon rubber;
(3) nano SiO on silicon rubber surface2Modifying the super-hydrophilic coating of the particles:
preparation of 50nm solid SiO by sol-gel method2Nano particles dispersed in TEOS alcohol solution by spin coating or dip-coating methodUniformly coating a layer of nano particles on the surface of the silicon rubber, then dropwise adding a small amount of ammonia water to crosslink the nano particles, and fixing the particle layer on the surface of the silicon rubber.
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| CN113198080B (en) * | 2021-04-08 | 2022-01-04 | 湖南万脉医疗科技有限公司 | Anti-condensation respirator pipeline and respirator |
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