CN118325343A - Preparation method of room temperature vulcanized silicone rubber for prosthetic fixation - Google Patents

Abstract

A preparation method of room temperature vulcanized silicone rubber for prosthetic fixation is disclosed, and a low-cost, simple preparation method and excellent performance silicone rubber product is developed. The improved silicone rubber has good elasticity, toughness, air permeability and mechanical properties. The preparation of silicone rubber includes four stages: dissolution of vinyl siloxane, filler, room temperature vulcanization and vacuum degassing. The specific preparation method includes the following steps: 1) dissolving vinyl siloxane in n-hexane and stirring until it is honey-like; 2) adding fumed silica, calcium carbonate and titanium dioxide to the honey-like vinyl siloxane and stirring and mixing thoroughly; 3) adding hydrogen-containing silicone oil (cross-linking agent) and placing it in a vacuum drying oven for the first vacuum degassing; 4) adding inhibitor and platinum catalyst for secondary vacuum degassing; 5) pouring the fluid silicone rubber semi-finished product on a flat mold for room temperature vulcanization reaction. Finally, a silicone rubber product for prosthetic fixation with good mechanical properties, air permeability and elastic toughness is obtained.

Description

Preparation method of room temperature vulcanized silicone rubber for prosthetic fixation

Technical Field

The invention relates to the technical field of polymer material synthesis and preparation, and in particular to a method for preparing room temperature vulcanized silicone rubber for prosthesis fixation.

Background technique

As an important polymer material, silicone rubber can provide a buffering effect on bone protrusions and sensitive parts due to its simple preparation process and excellent performance. Its high elasticity can make the residual limb fully contact and fix the shape, and its high tear resistance also increases its durability. These characteristics give silicone rubber a unique advantage in the manufacture of prostheses and can improve the comfort of users. Secondly, its good chemical stability ensures that it will not deform or age during use, thereby extending the service life of the prosthesis. Finally, its good electrical insulation performance can effectively prevent the conduction of current, thereby protecting the safety of prosthesis users. It is widely used in the medical field because of its many usage scenarios. It is widely used in the manufacture of various medical polymer materials, such as artificial organs, artificial joints, medical catheters, and silicone rubber straps for prosthetic fixation. Among them, medical catheters are the fastest-growing and most widely used products among medical silicone rubber products. Silicone rubber is also widely used in human body implants, such as artificial organs, dental impressions, cosmetic prostheses, medical catheters, and medical instrument sheaths, due to its non-toxic, odorless, and biological aging resistance. Silicone rubber is also widely used in the manufacture of medical devices, such as medical masks, nucleic acid testing kits, and extracorporeal membrane oxygenation (ECMO) machines. In addition, silicone rubber is often used for prosthetic fixation straps that need to be used for a long time because of its comfort, good mechanical properties, chemical stability, electrical insulation, and easy processing and manufacturing.

The present invention adopts room temperature vulcanization addition reaction to prepare silicone rubber, which has the advantages that the addition reaction is carried out at room temperature, and high temperature vulcanization is not required, thereby shortening the vulcanization time and reducing energy consumption; deep vulcanization, the addition reaction can be carried out simultaneously inside and on the surface of the silicone rubber product, thereby achieving deep vulcanization and improving the mechanical properties of the silicone rubber product. In addition to having advantages such as good toughness, the silicone rubber products prepared by room temperature vulcanization in this project also have good air permeability and moisture permeability, and can effectively remove sweat and moisture, thereby maintaining the comfort and health of the prosthesis user; the processing flow is simple, and prosthetic parts of various shapes and sizes can be made according to different needs, thereby meeting the needs of different patients; compared with other high-end materials, the price is more reasonable, and the overall cost performance is higher.

With the continuous development of medical technology, the requirements for the quality and performance of silicone rubber materials are also constantly increasing, and people's requirements for prosthetic-related products are also getting higher and higher, and they need to adapt to the needs of prosthetics of different age groups, different parts, and different functions. Therefore, the development of new and high-quality silicone rubber products can better adapt to diversified needs and meet the needs of different patients. In the future, prosthetic manufacturing will gradually develop in the direction of intelligence and personalization. As an important polymer material, silicone rubber has good processing and manufacturing performance, and can be intelligently and personalized by adding smart sensors, nanomaterials and other means. At present, the application of silicone rubber in the field of prosthetic manufacturing has been very extensive, but there are still many potential application areas to be expanded. For example, silicone rubber can be used to make auxiliary devices such as soft protective gear and orthotics, as well as medical devices and other fields that have yet to be developed. With the improvement of people's health awareness and the improvement of medical care level, the application of silicone rubber in the medical field will be more extensive. In short, there will be more research results and practical applications in the future, providing more possibilities for the development of the field of prosthetic manufacturing.

Summary of the invention

In view of the problems that there are many types of silicone rubber products, uneven performance, long-term monopoly of related core preparation technologies by foreign countries, and relatively expensive products, the present invention aims to prepare silicone rubber products with good elasticity, toughness, air permeability, moisture permeability and mechanical properties through a simple room temperature vulcanization method.

The technical solution of the present invention is specifically as follows:

The preparation method of room temperature vulcanized silicone rubber for prosthetic fixation is characterized by comprising the following steps:

(1) Dissolving raw materials: Dissolve vinyl siloxane in n-hexane and stir until it becomes honey-like;

(2) Filler: Add fumed silica, calcium carbonate and titanium dioxide into the honey-like vinyl siloxane and stir well to mix;

(3) Adding a cross-linking agent: dilute the hydrogenated silicone oil with n-hexane, quickly stir and mix with the raw materials, and place in a vacuum drying oven for vacuum degassing 3 to 5 times;

(4) Cross-linking and vacuum degassing: Add the inhibitor and platinum catalyst to n-hexane for dilution and quickly stir and mix with the raw materials, and place in a vacuum drying oven for vacuum degassing 3 to 5 times;

(5) Casting and vulcanization: Cast the fluid silicone rubber semi-finished product onto a flat mold, and then vulcanize and form it at room temperature to obtain a silicone rubber product.

Furthermore, in step (1), the mass ratio of vinyl siloxane to n-hexane is 1:1-4.

Furthermore, in step (2), the mass ratio of fumed silica to vinyl siloxane is 1:10-40.

Furthermore, in step (2), the mass ratio of calcium carbonate to vinyl siloxane is 1:1-20.

Furthermore, in step (2), the mass ratio of titanium dioxide to vinyl siloxane is 1:40-80.

Furthermore, in step (3), the mass ratio of hydrogenated silicone oil to vinyl siloxane is 1:10-40.

Furthermore, in the step (4), the ratio of the inhibitor is 1-50 μL per 10 g of vinyl siloxane.

Furthermore, in step (4), the ratio of platinum catalyst is 1-50 μL per 10 g of vinyl siloxane.

The main advantages of the present invention are:

The silicone rubber products prepared by room temperature vulcanization in this project not only have the advantages of good elasticity and toughness, but also have good air permeability and moisture permeability, and can effectively remove sweat and moisture, thereby maintaining the comfort and health of prosthetic users; the processing flow is simple, and prosthetic parts of various shapes and sizes can be made according to different needs, thus meeting the needs of different patients; compared with other high-end materials, the price is relatively reasonable, and the overall cost performance is high.

BRIEF DESCRIPTION OF THE DRAWINGS

In order to make the purpose, technical solution and beneficial effects of the present invention clearer, the present invention provides the following drawings:

FIG. 1 is a SEM image of the room temperature vulcanized silicone rubber used for prosthesis fixation before cross-linking in Example 1 of the present invention.

FIG. 2 is a SEM image of the cross-linked room temperature vulcanized silicone rubber used for prosthesis fixation in Example 1 of the present invention.

FIG. 3 is a physical picture of the room temperature vulcanized silicone rubber used for prosthesis fixation in Example 1 of the present invention.

FIG. 4 is a Fourier transform infrared spectrum of the room temperature vulcanized silicone rubber used for prosthesis fixation in Example 1 of the present invention.

FIG. 5 is a graph showing the mechanical tensile properties of the room temperature vulcanized silicone rubber (gauze) used for prosthetic fixation in Example 1 of the present invention.

FIG. 6 is a statistical table showing the water vapor permeability of the room temperature vulcanized silicone rubber used for prosthetic fixation in Example 1 of the present invention.

Detailed ways

The following examples are used to illustrate the present invention but are not intended to limit the scope of the present invention.

Example 1

(1) First, 800 mg of silica, 1 g of calcium carbonate, and 200 mg of titanium dioxide were ultrasonically dissolved in 25 mL of n-hexane until no flocs were evident.

(2) Add 10 g of vinyl siloxane to the mixed solvent in (1) and stir quickly and thoroughly until it becomes a honey-like state.

(3) Add 600 mg of hydrogenated silicone oil to 10 mL of n-hexane, dilute it, mix it with (2) and stir it rapidly. Place it in a vacuum drying oven and perform the initial vacuum degassing 3 to 5 times until no obvious bubbles are left.

(4) Add 25 μL of inhibitor and 25 μL of platinum catalyst to 25 mL of n-hexane, dilute and mix with (3), place in a vacuum drying oven and perform secondary vacuum degassing 3 to 5 times until no obvious bubbles are left.

(5) The fluid silicone rubber semi-finished product is poured onto a flat mold with gauze, and the silicone rubber product is obtained after vulcanization and molding at room temperature.

The scanning electron microscope (SEM) before cross-linking is shown in Figure 1, and no obvious bubbles are found, only a small amount of undissolved calcium carbonate and white carbon black particles; the scanning electron microscope (SEM) after cross-linking is shown in Figure 2, and bubbles generated by the addition reaction process appear in the field of view, proving that the silicone rubber is successfully cross-linked. Figure 3 is a real picture of room temperature vulcanized silicone rubber, and the sample is milky white elastic colloid. Figure 4 is a Fourier _infrared spectrum. The peaks at 2963 cm ^-1 , 1258 cm ^-1 and 787 cm ^-1 are the stretching vibration absorption peaks of the methyl group on Si- _CH3 , and the signal peaks at 1411 cm ^-1 and 706 cm ^-1 indicate the presence of Si- _C6H5 structure; the signal peaks at 1077 cm ^-1 and 1010 cm ^- 1 indicate that the polymer contains Si-O-Si structure. The side group contains phenyl groups, indicating that the product is a polymer containing methylsiloxane segments. Figure 5 is a mechanical tensile property test diagram of room temperature vulcanized silicone rubber (gauze) used for prosthetic fixation in Example 1 of the present invention. It can be seen from the figure that the lining cloth can significantly improve the tensile mechanical properties. FIG6 is a statistical table of water vapor permeability of two samples of room temperature vulcanized silicone rubber for prosthetic fixation in Example 1 of the present invention, which indicates that the product has stable and excellent air permeability and moisture permeability.

Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made in form and details without departing from the scope defined by the claims of the present invention.

Claims (8)

1. The preparation method of the room temperature vulcanized silicone rubber for fixing the artificial limb is characterized by comprising the following steps: comprises the following steps:

(1) Raw material dissolution: dissolving vinyl siloxane in n-hexane, and stirring to obtain honey;

(2) And (3) filling: adding fumed silica, calcium carbonate and titanium dioxide into honey-like vinyl siloxane, and fully stirring and mixing;

(3) Adding a cross-linking agent: adding hydrogen-containing silicone oil into n-hexane, diluting, rapidly stirring and mixing with the raw materials, and placing into a vacuum drying oven for vacuum defoaming for 3-5 times;

(4) Crosslinking and vacuum defoamation: adding a polymerization inhibitor and a platinum catalyst into n-hexane, diluting, rapidly stirring and mixing with raw materials, and placing into a vacuum drying oven for vacuum defoaming for 3-5 times;

(5) Pouring and vulcanizing: pouring the fluid-shaped semi-finished silicone rubber product on a flat plate mold, and obtaining the silicone rubber product after room temperature vulcanization molding.

2. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: the mass ratio of the vinyl siloxane to the n-hexane in the step (1) is 1: 1-4.

3. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: the mass ratio of the gas-phase white carbon black to the vinyl siloxane in the step (2) is 1: 10-40.

4. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: the mass ratio of the calcium carbonate to the vinyl siloxane in the step (2) is 1: 1-20.

5. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: the mass ratio of the titanium dioxide to the vinyl siloxane in the step (2) is 1: 40-80 parts.

6. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: the mass ratio of the hydrogen-containing silicone oil to the vinyl siloxane in the step (3) is 1: 10-40.

7. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: and (3) adding 1-50 mu L of polymerization inhibitor into the reaction kettle in the step (4) every 10 g vinyl siloxane.

8. The method for preparing room temperature vulcanized silicone rubber for fixing artificial limb according to claim 1, wherein: and (3) adding 1-50 mu L of platinum catalyst in the step (4) every 10 g vinyl siloxane.