CN113398318B - Preparation method of medical adhesive and medical adhesive - Google Patents
Preparation method of medical adhesive and medical adhesive Download PDFInfo
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- CN113398318B CN113398318B CN202110657309.8A CN202110657309A CN113398318B CN 113398318 B CN113398318 B CN 113398318B CN 202110657309 A CN202110657309 A CN 202110657309A CN 113398318 B CN113398318 B CN 113398318B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/02—Surgical adhesives or cements; Adhesives for colostomy devices containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/06—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The application relates to the field of adhesives, and particularly discloses a preparation method of a medical adhesive and the medical adhesive. The preparation method of the medical adhesive comprises the following steps: mixing 107 room temperature vulcanized silicone rubber, white carbon black and dimethyl diethoxy silane to form rubber compound; repeatedly mixing the rubber compound for 6-8 times to obtain a medical adhesive base material A; drying to obtain a medical adhesive base material B; repeatedly mixing the medical adhesive base material B for 3-5 times to obtain a medical adhesive base material C; reacting the medical adhesive base material C for 2.8-3.2h at 140 +/-2 ℃, and introducing nitrogen in the whole reaction process; adding methyl triacetoxysilane, reacting at 65 + -2 deg.C for 0.4-0.6 hr, introducing nitrogen gas during the reaction, and discharging to obtain the final product. The preparation method has clear flow and strong operability, and the prepared medical adhesive has better stability.
Description
Technical Field
The application relates to the technical field of adhesives, in particular to a preparation method of a medical adhesive and the medical adhesive.
Background
The subcutaneous implantation contraception method is a novel contraception method and has been popularized and used all over the world. The contraceptive method is that a drug core made of a certain dosage of progestogen is placed in a silica gel tube to form a contraceptive implant, and then the contraceptive implant is embedded under the skin to slowly release a small amount of progestogen, thereby playing the contraceptive role. The production process of the contraceptive implant comprises the following steps: producing a medicine core; producing a silicone tube; using a medical adhesive to seal one end of the silicone tube; filling the medicine core into a silica gel tube; the other end of the silicone tube is blocked by medical adhesive.
In the contraceptive implant, the main component of the drug core is estrogen medicine, and the adhesive for plugging the two ends of the silicone tube generally adopts medical silicone or polysiloxane. When the contraceptive implant is subcutaneously implanted, the effective contraceptive period is 4 years, and thus the medical adhesive used needs to have better stability.
Aiming at the related technologies, the production method for effectively improving the stability of the medical adhesive has very important significance.
Disclosure of Invention
In order to provide a production method capable of improving the stability of a medical adhesive, the application provides a preparation method of the medical adhesive and the medical adhesive.
In a first aspect, the present application provides a method for preparing a medical adhesive, which adopts the following technical scheme:
a method of preparing a medical adhesive comprising the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.2-0.5 mm, adding 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding white carbon black and dimethyl diethoxy silane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller, and mixing the 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyl diethoxy silane to form mixed rubber;
s2, when the rubber compound covers the whole roller, shoveling the rubber compound down and placing the rubber compound in a container, and shoveling the rubber compound in the container into the space between the two rollers of the open mill again to continue mixing;
s3, repeating the step S2 for 6-8 times to obtain a medical adhesive base material A;
s4, drying the medical adhesive base material A at 140 +/-2 ℃ for 55-65min to obtain a medical adhesive base material B;
s5, opening the open mill, adjusting the distance between the two rollers of the open mill to be 0.2-0.5 mm, and shoveling the medical adhesive base material B into the space between the two rollers of the open mill for continuous mixing;
s6, when the medical adhesive base material B covers the whole roller, shoveling the medical adhesive base material B down and placing the medical adhesive base material B in a container, and shoveling the medical adhesive base material B in the container into the space between the two rollers of the open mill again to continue mixing;
s7, repeating the step S6 for 3-5 times to obtain a medical adhesive base material C;
s8, putting the medical adhesive base material C into a reaction kettle, reacting for 2.8-3.2h under the condition that the internal temperature is 140 +/-2 ℃, and introducing nitrogen in the whole reaction process;
s9, adding a cross-linking agent into the reaction kettle, continuing to react for 0.4-0.6h under the condition that the internal temperature is 65 +/-2 ℃, introducing nitrogen in the whole reaction process, and discharging to obtain the finished product of the medical adhesive.
By adopting the technical scheme, the preparation method has clear flow and strong operability, and the adhesion thickness of the mixture on the surface of the roller is controlled by adjusting the distance between the two rollers of the open mill, so that all components are fully mixed. By repeating the operation of step S2 a plurality of times, the degree of mixing between the components is further improved, and the raw materials are sufficiently reacted. The medical adhesive base material A is dried and then mixed again, so that the mixing degree of the raw material components is further improved, and the stability of the prepared medical adhesive is improved. The preparation method has reasonable steps, and the prepared medical adhesive has higher stability by strictly controlling parameters of the steps.
Preferably, in the S9, the addition amount of the cross-linking agent is 6.8-7.2% of the weight of the traditional Chinese medicine adhesive base material C added into the reaction kettle in the S8.
By adopting the technical scheme, when the usage amount of the cross-linking agent is controlled in the range, the cross-linking agent can fully participate in the reaction, so that linear molecules in the raw materials are fully connected, and the stability of the prepared medical adhesive is improved.
Preferably, the weighing steps of the weight of the traditional Chinese medicine adhesive base material C put into the reaction kettle in S8 are as follows: the medical adhesive base material C is shoveled into a stainless steel container, the stainless steel container and the medical adhesive base material C are weighed integrally and recorded as M1, the medical adhesive base material C is shoveled into a reaction kettle, the stainless steel container and the medical adhesive base material C adhered in the stainless steel container are weighed integrally again and recorded as M2, the weight of the medical adhesive base material C put into the reaction kettle in S8 is recorded as M, and then M is M1-M2.
By adopting the technical scheme, the weight of the traditional Chinese medicine adhesive base material C put into the reaction kettle in S8 can be obtained more accurately, so that the adding precision of the cross-linking agent is improved according to the scientific proportion, and the stability of the prepared medical adhesive is improved.
Preferably, in S9, the crosslinking agent is methyltriacetoxysilane.
By adopting the technical scheme, when the methyl triacetoxy silane is used as the cross-linking agent, the prepared medical adhesive has better stability, and the viscosity before and after aging is lower after aging test.
Preferably, in the S8 and S9, the rotation speed is set to 150-180r/min during the reaction process.
By adopting the technical scheme, the stability of the prepared medical adhesive can be improved by controlling the reaction rotating speed within the range.
Preferably, in the S8 and S9, the nitrogen flow rate is 1-2L/min.
By adopting the technical scheme, in the reaction process, when the nitrogen flow is in the range, the prepared medical adhesive has better stability, and the viscosity before and after aging is lower after aging test.
Preferably, in S1, the viscosity of the 107 room temperature vulcanized silicone rubber at 25 ℃ is 2000-7000mPa.s, the surface vulcanization time is less than or equal to 2.0h, and the total number of bacteria, yeasts and molds is less than or equal to 100 CFU/g.
Preferably, in S1, the dimethyl diethoxysilane has a pH of 6.0-8.0 and a refractive index nD 201.3790-1.3820, specific gravity d4 20Is 0.82-0.88g/cm3。
By adopting the technical scheme, the medical adhesive prepared from the raw materials has better stability, and the viscosity before and after aging is lower after aging test.
In a second aspect, the present application provides a medical adhesive, which adopts the following technical scheme:
a medical adhesive prepared by the method of preparing a medical adhesive according to any one of claims 1 to 8.
By adopting the technical scheme, the medical adhesive is free of adding heavy metal materials as a catalyst in the preparation process, is harmless to human bodies, has good stability, and can be used for more than 4 years at normal temperature.
Preferably, the medical adhesive is used for plugging two ends of the contraceptive implant silicone tube.
Through adopting above-mentioned technical scheme, use the medical adhesive of this application behind shutoff silicone tube both ends, because this application medical adhesive has better stability, guaranteed that the circumstances that the medicine core was revealed can not appear in the term of service of contraception implanting agent takes place to the contraception effect of contraception implanting agent has been guaranteed.
In summary, the present application has the following beneficial effects:
1. the preparation method has clear flow and strong operability, and improves the stability of the prepared medical adhesive through scientific operation steps and technological parameters;
2. the preparation method of the application does not add heavy metal materials, so that the prepared medical adhesive is harmless to human bodies;
3. the medical adhesive prepared by the application can be used for blocking two ends of the contraceptive implant silicone tube, and has better stability, so that the occurrence of the situation that the medicine core of the contraceptive implant leaks in the service life is reduced, and the contraceptive effect of the contraceptive implant is ensured.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the examples of the present application are commercially available, except for the following specific descriptions:
white carbon black is collected from EVONUK (winning group), brand: r106;
the dimethyldiethoxysilane is obtained from chemical reagents of national drug group, Inc.;
107 room temperature vulcanized silicone rubber is obtained from Shanghai resin factory, Inc. with the model number of 107;
the methyltriacetoxysilane was collected from New materials of New blue sky, Inc. of Hubei;
the ethyl triacetoxysilane is collected from New materials of New blue sky, Inc. of Hubei;
the open mill is made of the model XSK-l60A of Wuxi Ming big rubber and plastic machinery company Limited.
Examples
Example 1
A preparation method of a medical adhesive comprises the following steps:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.5 mm, adding 998g of 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding 89g of white carbon black and 11.5g of dimethyldiethoxysilane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller (namely the 107 room temperature vulcanized silicone rubber covers the position 3cm away from the two ends of the roller), and mixing 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyldiethoxysilane to form mixed rubber;
s2, when the rubber compound covers the whole roller (namely the rubber compound covers the position 3cm away from the two ends of the roller), shoveling the rubber compound down and placing the rubber compound in a container, and shoveling the rubber compound in the container into the space between the two rollers of the open mill again to continue mixing;
s3, repeating the step S2 for 6 times to obtain a medical adhesive base material A;
s4, drying the medical adhesive base material A at 140 +/-2 ℃ for 55min to obtain a medical adhesive base material B;
s5, opening the open mill, adjusting the distance between the two rollers of the open mill to be 0.5 mm, and shoveling the medical adhesive base material B into the space between the two rollers of the open mill for continuous mixing;
s6, when the medical adhesive base material B covers the whole roller (namely the medical adhesive base material B covers the position 3cm away from the two ends of the roller), the medical adhesive base material B is shoveled and placed in a container, and then the medical adhesive base material B in the container is shoveled into the space between the two rollers of the open mill again to be continuously mixed;
s7, repeating the step S6 for 3 times to obtain a medical adhesive base material C;
s8, shoveling the medical adhesive base material C into a stainless steel container (the specification of the stainless steel container is 26cm x 20cm x 3cm, and the weight is 800g), shoveling the stainless steel container and the medical adhesive base material C into a reaction kettle, reacting for 2.8 hours at the internal temperature of 140 +/-2 ℃ and the stirring speed of 120r/min, introducing nitrogen gas into the whole reaction process at the nitrogen flow rate of 0.5L/min, shoveling the medical adhesive base material C into the reaction kettle, shoveling the medical adhesive base material C into the stainless steel container and the medical adhesive base material C adhered to the stainless steel container again, shoveling the medical adhesive base material C into the reaction kettle into M2 and M2 897.4g, shoveling the medical adhesive base material C into the reaction kettle into M, and weighing the medical adhesive base material C into M1-M2-897.3 g;
s9, adding 53.8g (Mx 6.0%) of a cross-linking agent into the reaction kettle, wherein the cross-linking agent is ethyl triacetoxysilane, continuously reacting for 0.4h under the conditions that the internal temperature is 65 ℃ and the stirring speed is 120r/min, introducing nitrogen in the whole reaction process, and the nitrogen flow rate is 0.5L/min, and discharging to obtain the finished product of the medical adhesive.
Examples 2 to 5
A method for producing a medical adhesive, which is different from example 1 in that the amounts of the respective raw materials used are shown in Table 1, and the numerical values of M1, M2 and M are shown in Table 2.
TABLE 1 usage amounts (g) of respective raw materials in examples 1 to 5
TABLE 2 numerical values (g) of M1, M2, M in examples 1 to 5
Examples 6 to 9
A method for producing a medical adhesive, which is different from example 1 in that the amounts of the respective raw materials used are shown in Table 3, and the numerical values of M1, M2 and M are shown in Table 4.
TABLE 3 usage amounts (g) of respective raw materials in examples 1, 6 to 9
TABLE 4 values (g) of M1, M2, M in examples 1, 6-9
Example 10
A preparation method of a medical adhesive is different from that of example 7 in that a crosslinking agent used is methyl triacetoxysilane, the addition amount of the crosslinking agent is 7.0% of the weight of a traditional Chinese medicine adhesive base material C added into a reaction kettle in S8, and the numerical values of M1, M2 and M are shown in Table 5.
Examples 11 to 18
A method for producing a medical adhesive, which is different from example 10 in that the rotational speed and the nitrogen flow rate during the reaction in S8 and S9 are shown in Table 6 and the numerical values of M1, M2 and M are shown in Table 5.
TABLE 5 values (g) for M1, M2, M in examples 10-18
TABLE 6 rotation speed and nitrogen flow rate during the reactions in examples 10-18
Example 19
A method for preparing a medical adhesive, which is different from example 1 in that it comprises the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.2 mm, adding 998g of 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding 89g of white carbon black and 11.5g of dimethyl diethoxy silane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller (namely the 107 room temperature vulcanized silicone rubber covers the position 3cm away from the two ends of the roller), and mixing 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyl diethoxy silane to form mixed rubber;
s2, when the rubber compound covers the whole roller (namely the rubber compound covers the position 3cm away from the two ends of the roller), shoveling the rubber compound down and placing the rubber compound in a container, and shoveling the rubber compound in the container into the space between the two rollers of the open mill again to continue mixing;
s3, repeating the step S2 for 8 times to obtain a medical adhesive base material A;
s4, drying the medical adhesive base material A at 140 +/-2 ℃ for 65min to obtain a medical adhesive base material B;
s5, opening the open mill, adjusting the distance between the two rollers of the open mill to be 0.2 mm, and shoveling the medical adhesive base material B into the space between the two rollers of the open mill for continuous mixing;
s6, when the medical adhesive base material B covers the whole roller (namely the medical adhesive base material B covers the position 3cm away from the two ends of the roller), the medical adhesive base material B is shoveled and placed in a container, and then the medical adhesive base material B in the container is shoveled into the space between the two rollers of the open mill again to be continuously mixed;
s7, repeating the step S6 for 5 times to obtain a medical adhesive base material C;
s8, shoveling the medical adhesive base material C into a stainless steel container (the specification of the stainless steel container is 26cm x 20cm x 3cm, and the weight is 800g), shoveling the stainless steel container and the medical adhesive base material C into a reaction kettle, reacting for 3.2h under the conditions that the internal temperature is 140 +/-2 ℃ and the stirring speed is 120r/min, introducing nitrogen gas into the whole reaction process at the nitrogen flow rate of 0.5L/min, shoveling the medical adhesive base material C into the reaction kettle, shoveling the medical adhesive base material C into the stainless steel container and the medical adhesive base material C adhered to the stainless steel container again, shoveling the medical adhesive base material C into the reaction kettle into M2 and M2 898.2g, shoveling the medical adhesive base material C into the reaction kettle into M, and weighing the medical adhesive base material C into M1-M2-899.9 g;
s9, adding 54.0g (Mx 6.0%) of a cross-linking agent into the reaction kettle, wherein the cross-linking agent is ethyl triacetoxysilane, continuously reacting for 0.6h under the conditions that the internal temperature is 65 ℃ and the stirring speed is 120r/min, introducing nitrogen in the whole reaction process, and the nitrogen flow rate is 0.5L/min, and discharging to obtain the finished product of the medical adhesive.
Comparative example
Comparative example 1
A method for preparing an adhesive, which is different from example 1 in that it comprises the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.5 mm, adding 998g of 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding 89g of white carbon black and 11.5g of dimethyldiethoxysilane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller (namely the 107 room temperature vulcanized silicone rubber covers the position 3cm away from the two ends of the roller), and mixing 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyldiethoxysilane to form mixed rubber;
s2, when the rubber compound covers the whole roller (namely the rubber compound covers the position 3cm away from the two ends of the roller), shoveling the rubber compound down and placing the rubber compound in a container, shoveling the rubber compound in the container into the space between the two rollers of the open mill again for continuous mixing to obtain a medical adhesive base material A;
s3, shoveling the medical adhesive base material A into a stainless steel container (the specification of the stainless steel container is 26cm by 20cm by 3cm, and the weight is 800g), shoveling the stainless steel container and the medical adhesive base material A into a reaction kettle, reacting for 2.8 hours under the conditions that the internal temperature is 140 +/-2 ℃ and the stirring speed is 120r/min, introducing nitrogen gas into the whole reaction process at the nitrogen flow rate of 0.5L/min, shoveling the medical adhesive base material A adhered to the stainless steel container and the stainless steel container into the reaction kettle again, shoveling the medical adhesive base material A into the reaction kettle into M2 and M2 899.6g, shoveling the weight of the medical adhesive base material A put into the reaction kettle into M, and then weighing the M1-M2-896.8 g;
s4, adding 53.8g (Mx 6.0%) of a cross-linking agent into the reaction kettle, wherein the cross-linking agent is ethyl triacetoxysilane, continuously reacting for 0.4h under the conditions that the internal temperature is 65 ℃ and the stirring speed is 120r/min, introducing nitrogen in the whole reaction process, and the nitrogen flow rate is 0.5L/min, and discharging to obtain the finished product of the medical adhesive.
Comparative example 2
A method for preparing an adhesive, which is different from example 1 in that it comprises the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.5 mm, adding 998g of 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding 89g of white carbon black and 11.5g of dimethyldiethoxysilane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller (namely the 107 room temperature vulcanized silicone rubber covers the position 3cm away from the two ends of the roller), and mixing 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyldiethoxysilane to form mixed rubber;
s2, when the rubber compound covers the whole roller (namely the rubber compound covers the position 3cm away from the two ends of the roller), shoveling the rubber compound down and placing the rubber compound in a container, and shoveling the rubber compound in the container into the space between the two rollers of the open mill again to continue mixing;
s3, repeating the step S2 for 6 times to obtain a medical adhesive base material A;
s4, shoveling the medical adhesive base material A into a stainless steel container (the specification of the stainless steel container is 26cm by 20cm by 3cm, and the weight is 800g), shoveling the stainless steel container and the medical adhesive base material A into a reaction kettle, reacting for 2.8 hours under the conditions that the internal temperature is 140 +/-2 ℃ and the stirring speed is 120r/min, introducing nitrogen gas into the whole reaction process at the nitrogen flow rate of 0.5L/min, shoveling the medical adhesive base material A adhered to the stainless steel container and the stainless steel container into the reaction kettle again, shoveling the medical adhesive base material A into the reaction kettle into M2 and M2 898.9g, shoveling the weight of the medical adhesive base material A put into the reaction kettle into M, and then weighing the M1-M2-898.4 g;
s5, adding 53.9g (Mx 6.0%) of a cross-linking agent into the reaction kettle, wherein the cross-linking agent is ethyl triacetoxysilane, continuously reacting for 0.4h under the conditions that the internal temperature is 65 ℃ and the stirring speed is 120r/min, introducing nitrogen in the whole reaction process, and the nitrogen flow rate is 0.5L/min, and discharging to obtain the finished product of the medical adhesive.
Comparative example 3
A method for preparing an adhesive, which is different from example 1 in that it comprises the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.5 mm, adding 998g of 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding 89g of white carbon black and 11.5g of dimethyldiethoxysilane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller (namely the 107 room temperature vulcanized silicone rubber covers the position 3cm away from the two ends of the roller), and mixing 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyldiethoxysilane to form mixed rubber;
s2, when the rubber compound covers the whole roller (namely the rubber compound covers the position 3cm away from the two ends of the roller), shoveling the rubber compound down and placing the rubber compound in a container, shoveling the rubber compound in the container into the space between the two rollers of the open mill again for continuous mixing to obtain a medical adhesive base material A;
s3, drying the medical adhesive base material A at 140 +/-2 ℃ for 55min to obtain a medical adhesive base material B;
s4, opening the open mill, adjusting the distance between the two rollers of the open mill to be 0.5 mm, and shoveling the medical adhesive base material B into the space between the two rollers of the open mill for continuous mixing;
s5, when the medical adhesive base material B covers the whole roller (namely the medical adhesive base material B covers the position 3cm away from the two ends of the roller), shoveling the medical adhesive base material B down and placing the medical adhesive base material B in a container, shoveling the medical adhesive base material B in the container into the two rollers of the open mill again and continuously mixing to obtain a medical adhesive base material C;
s6, shoveling the medical adhesive base material C into a stainless steel container (the specification of the stainless steel container is 26cm x 20cm x 3cm, and the weight is 800g), shoveling the stainless steel container and the medical adhesive base material C into a reaction kettle, reacting for 2.8 hours at the internal temperature of 140 +/-2 ℃ and the stirring speed of 120r/min, introducing nitrogen gas into the whole reaction process at the nitrogen flow rate of 0.5L/min, shoveling the medical adhesive base material C into the reaction kettle, shoveling the medical adhesive base material C into the stainless steel container and the medical adhesive base material C adhered to the stainless steel container again, shoveling the medical adhesive base material C into the reaction kettle into M2 and M2 895.3g, shoveling the medical adhesive base material C into the reaction kettle into M, and weighing the medical adhesive base material C into M1-M2-895.9 g;
s7, adding 53.8g (Mx 6.0%) of a cross-linking agent into the reaction kettle, wherein the cross-linking agent is ethyl triacetoxysilane, continuously reacting for 0.4h under the conditions that the internal temperature is 65 ℃ and the stirring speed is 120r/min, introducing nitrogen in the whole reaction process, and the nitrogen flow rate is 0.5L/min, and discharging to obtain the finished product of the medical adhesive.
Performance test
The medical adhesives prepared in examples 1 to 19 and comparative examples 1 to 3 were respectively used as test objects and tested for stability by the following methods: and (3) placing the test sample in an oven at 80 ℃ for aging treatment for 14d, testing the ratio of the viscosity before aging treatment to the viscosity after aging treatment, and if the ratio of the viscosity before aging treatment to the viscosity after aging treatment is less than or equal to 2.5, the medical adhesive is stable in a human body for 4 years, and the test results are shown in the following table 7.
Table 7 stability test results
As can be seen from the test data in table 7: the medical adhesive prepared by the preparation method has better stability, and the viscosity ratio of the medical adhesive before and after aging is lower than 1.27 after aging test, so that the medical adhesive prepared by the embodiment of the application has better viscosity after being used in a human body for 4 years, and the medical adhesive prepared by the embodiment of the application has better stability and can be applied to the sealing end of a contraceptive implant silicone tube.
In combination with example 1 and comparative examples 1 to 3, and table 7, it can be seen that in comparative examples 1 to 3, the step of example 1 of the present application is partially omitted, which results in the stability of the prepared medical adhesive being lowered, thereby indicating that the medical adhesive with better stability can be prepared by the preparation method of the medical adhesive of the present application, and the medical adhesive obtained by the preparation method of the present application can provide better contraceptive effect within the service life when applied to the end of the silicone tube of the contraceptive implant.
The difference between example 1 and examples 6-9 is that the crosslinking agent is used differently, and it can be seen from the data in Table 7 that when the amount of the crosslinking agent added is 6.8-7.2% of the weight of the traditional Chinese medicine adhesive base C added into the reaction kettle in S8, the prepared medical adhesive has better stability.
The difference between example 7 and example 10 is that in example 10, methyltriacetoxysilane was used as a crosslinking agent, and it can be seen from the data in Table 7 that when methyltriacetoxysilane was used as a crosslinking agent, the stability of the resulting medical adhesive can be significantly improved.
The difference between example 10 and examples 11 to 14 is that the rotation speeds of the reactions in S8 and S9 are different, and it can be seen from the data in Table 7 that when the rotation speed is set to 150-180r/min during the reaction process, the stability of the prepared medical adhesive can be significantly improved, and the viscosity of the medical adhesive before and after aging is relatively low after the aging test.
The difference between example 12 and examples 15 to 18 is that the nitrogen gas flow rates in S8 and S9 were different, and it is understood from the data in Table 7 that the stability of the resulting medical adhesive was remarkably improved when the nitrogen gas flow rate was 1 to 2L/min.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A method for preparing a medical adhesive, comprising the steps of:
s1, opening the open mill, adjusting the distance between two rollers of the open mill to be 0.2-0.5 mm, adding 107 room temperature vulcanized silicone rubber between the two rollers of the open mill, adding white carbon black and dimethyl diethoxy silane for mixing when the 107 room temperature vulcanized silicone rubber covers the whole roller, and mixing the 107 room temperature vulcanized silicone rubber, the white carbon black and the dimethyl diethoxy silane to form mixed rubber;
s2, when the rubber compound covers the whole roller, shoveling the rubber compound down and placing the rubber compound in a container, and shoveling the rubber compound in the container into the space between the two rollers of the open mill again to continue mixing;
s3, repeating the step S2 for 6-8 times to obtain a medical adhesive base material A;
s4, drying the medical adhesive base material A at 140 +/-2 ℃ for 55-65min to obtain a medical adhesive base material B;
s5, opening the open mill, adjusting the distance between the two rollers of the open mill to be 0.2-0.5 mm, and shoveling the medical adhesive base material B into the space between the two rollers of the open mill for continuous mixing;
s6, when the medical adhesive base material B covers the whole roller, shoveling the medical adhesive base material B down and placing the medical adhesive base material B in a container, and shoveling the medical adhesive base material B in the container into the space between the two rollers of the open mill again to continue mixing;
s7, repeating the step S6 for 3-5 times to obtain a medical adhesive base material C;
s8, putting the medical adhesive base material C into a reaction kettle, reacting for 2.8-3.2h under the condition that the internal temperature is 140 +/-2 ℃, and introducing nitrogen in the whole reaction process;
s9, adding a cross-linking agent into the reaction kettle, continuously reacting for 0.4-0.6h under the condition that the internal temperature is 65 +/-2 ℃, introducing nitrogen in the whole reaction process, and discharging to obtain a finished medical adhesive;
in the S9, the addition amount of the cross-linking agent is 6.8-7.2% of the weight of the traditional Chinese medicine adhesive base material C added into the reaction kettle in the S8.
2. The method for preparing the medical adhesive according to claim 1, wherein the step of weighing the traditional Chinese medicine adhesive base material C put into the reaction kettle in S8 comprises the following steps: the medical adhesive base material C is shoveled into a stainless steel container, the stainless steel container and the medical adhesive base material C are weighed integrally and recorded as M1, the medical adhesive base material C is shoveled into a reaction kettle, the medical adhesive base material C adhered in the stainless steel container and the stainless steel container is weighed integrally and recorded as M2, the weight of the medical adhesive base material C put into the reaction kettle in S8 is recorded as M, and then M = M1-M2.
3. The method for preparing a medical adhesive according to claim 1, wherein in S9, the crosslinking agent is methyltriacetoxysilane.
4. The method as claimed in claim 1, wherein the rotation speed during the reaction is set to 150-180r/min in S8 and S9.
5. The method for preparing a medical adhesive according to claim 1, wherein a flow rate of nitrogen gas in S8 and S9 is 1-2L/min.
6. The method for preparing the medical adhesive according to claim 1, wherein in the step S1, the viscosity of the 107 room temperature vulcanized silicone rubber at 25 ℃ is 2000-7000mPa.s, the surface vulcanization time is less than or equal to 2.0h, and the total number of bacteria, yeasts and molds is less than or equal to 100 CFU/g.
7. The method for preparing a medical adhesive according to claim 1, wherein in the S1, the dimethyldiethoxysilane has a pH of 6.0 to 8.0 and a refractive index nD 201.3790-1.3820, specific gravity d4 20Is 0.82-0.88g/cm3。
8. A medical adhesive, characterized in that it is prepared by the process for the preparation of a medical adhesive according to any one of claims 1 to 7.
9. The medical adhesive according to claim 8, wherein said medical adhesive is used for sealing off both ends of a contraceptive implant silicone tube.
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