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CN-121991517-A - Medical silica gel sealing ring material and preparation method thereof

CN121991517ACN 121991517 ACN121991517 ACN 121991517ACN-121991517-A

Abstract

The invention discloses a medical silica gel sealing ring material and a preparation method thereof, and relates to the field of silica gel materials. The invention relates to a medical silica gel sealing ring material, which is prepared by uniformly mixing and reacting mica powder, phytic acid, diglycidyl ether and allyl glycidyl ether to obtain modified mica powder, reacting 4- (2-amino ethyl) phenylboric acid and 3,3' -dihydroxyl- [1,1' -biphenyl ] -4,4' -dicarboxaldehyde to obtain a graft, reacting vinyl silicone oil, thioglycerol and methacryloyl ethyl sulfobetaine to obtain modified silica gel, and uniformly mixing and reacting the modified silica gel, the modified mica powder and the graft to obtain the medical silica gel sealing ring material. The medical silica gel sealing ring material prepared by the invention has excellent flame retardance, ageing resistance, antifouling property and mechanical property.

Inventors

  • ZHANG WEI
  • GAO ZHIYUAN
  • FENG ZHIJUN

Assignees

  • 江苏泰胜康医疗科技有限公司

Dates

Publication Date
20260508
Application Date
20260326

Claims (8)

  1. 1. The medical silica gel sealing ring material is characterized by being prepared by uniformly mixing and reacting modified silica gel, modified mica powder and grafts; The modified silica gel is obtained by reacting vinyl silicone oil, thioglycerol and methacryloyl ethyl sulfobetaine; the modified mica powder is obtained by uniformly mixing and reacting mica powder, phytic acid, diglycidyl ether and allyl glycidyl ether; the graft is prepared by reacting 4- (2-aminoethyl) phenylboronic acid with 3,3' -dihydroxy- [1,1' -biphenyl ] -4,4' -dicarboxaldehyde.
  2. 2. The preparation method of the medical silica gel sealing ring material is characterized by comprising the following preparation steps: (1) Uniformly mixing mica powder, phytic acid, diglycidyl ether, allyl glycidyl ether and deionized water according to the mass ratio of 1 (0.4-0.6) (0.1-0.2) (0.05-0.07) (25-35), carrying out ultrasonic treatment at 55-65 ℃ for 23-25 hours, centrifuging, washing with deionized water for 3-5 times, and drying at 55-65 ℃ for 11-13 hours to obtain modified mica powder; (2) Uniformly mixing 4- (2-aminoethyl) phenylboronic acid, 3' -dihydroxyl- [1,1' -biphenyl ] -4,4' -dicarboxaldehyde, a 3A molecular sieve and absolute ethyl alcohol according to the mass ratio of 1 (0.7-0.8) (0.2-0.3) (15-25), stirring at 20-30 ℃ and 100-300 rpm for 25-35 min, taking out the molecular sieve, carrying out vacuum suction filtration, adding a phosphoric acid solution, heating to 65-75 ℃ and refluxing for 2-4 h, adding deionized water 70-80 times the mass of 4- (2-aminoethyl) phenylboronic acid, regulating the pH, continuously stirring for 25-35 min, extracting and separating liquid, taking an organic phase, adding sodium sulfate for drying, adding an ethyl oxalate solution, standing and precipitating, filtering, adding deionized water 70-80 times the mass of 4- (2-aminoethyl) phenylboronic acid, continuously stirring for 25-35 min, extracting and separating liquid, adding the organic phase into sodium sulfate for drying and filtering, and carrying out rotary evaporation to obtain a graft; (3) Uniformly mixing vinyl silicone oil, thioglycerol, methacryloyl ethyl sulfobetaine and tetrahydrofuran according to the mass ratio of (0.07-0.09) (0.1-0.2) (7-9), stirring for 25-35 min at 20-30 ℃ and 100-300 rpm, adding an initiator with the mass of 0.0001-0.0002 times of that of the vinyl silicone oil, stirring for 11-13 h in a nitrogen atmosphere at 65-75 ℃ and 200-400 rpm, pouring the mixture into absolute ethyl alcohol with the mass of 15-17 times of that of the vinyl silicone oil, standing for precipitation, filtering, adding tetrahydrofuran for dissolving, repeatedly precipitating for 2-4 times, and drying for 23-25 h at 50-60 ℃ to obtain modified silica gel; (4) Uniformly mixing modified silica gel, modified mica powder, grafts and vulcanizing agent according to the mass ratio of 1 (0.03-0.05) (0.06-0.08) (0.005-0.007), mixing for 15-25 min at 20-30 ℃ by an internal mixer, placing in an iron mold, pre-vulcanizing for 5-15 min at 170-180 ℃ and vulcanizing for 1-3 h at 195-205 ℃ to obtain the medical silica gel sealing ring material.
  3. 3. The preparation method of the medical silica gel sealing ring material according to claim 2, wherein the mass fraction of the phosphoric acid solution in the step (2) is 80% -90%, and the addition amount is 5-15 times of the mass of the 4- (2-aminoethyl) phenylboronic acid.
  4. 4. The method for preparing a medical silica gel sealing ring material according to claim 2, wherein the pH adjustment in the step (2) is performed by adjusting the pH to 8-9 with sodium bicarbonate.
  5. 5. The method for preparing the medical silica gel sealing ring material according to claim 2, wherein the concentration of the ethyl oxalate solution in the step (2) is 0.011-0.013 g/mL, and the addition amount is 70-80 times of the mass of 4- (2-aminoethyl) phenylboronic acid.
  6. 6. The method for preparing a medical silica gel sealing ring material according to claim 2, wherein ethyl acetate is used as the extraction liquid in the step (2), and the addition amount of the ethyl acetate is 70-80 times of the mass of 4- (2-aminoethyl) phenylboronic acid.
  7. 7. The method for preparing a medical silicone gasket material according to claim 2, wherein the initiator in the step (3) is azobisisobutyronitrile.
  8. 8. The method for preparing a medical silica gel sealing ring material according to claim 2, wherein the vulcanizing agent in the step (4) is 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.

Description

Medical silica gel sealing ring material and preparation method thereof Technical Field The invention relates to the field of silica gel materials, in particular to a medical silica gel sealing ring material and a preparation method thereof. Background With rapid development of science and technology and continuous progress of medical science, medical level is remarkably improved, a plurality of difficult and complicated diseases can be timely found and effectively treated, and also, higher requirements are put on auxiliary treatment instruments, and medical instrument requirements with excellent biological characteristics are increased, so that development of biopolymer material industry and medical instrument industry is promoted. The medical silica gel sealing ring is a key component in medicine packaging and medical appliances, and the performance of the medical silica gel sealing ring is directly related to the safety of liquid medicine and the reliability of equipment. At present, most of the mainstream medical silica gel sealing rings adopt peroxide vulcanized methyl vinyl silicone rubber, and although the main stream medical silica gel sealing rings have good biocompatibility and temperature resistance, obvious defects still exist. Firstly, in the long-term and repeated high-pressure steam sterilization process, the problem of thermal oxidative aging is prominent, so that the material is gradually hardened and cracked, the oxidation aging resistance is insufficient, and the service life is shortened. Secondly, the existing materials have contradiction between mechanical property and elasticity, namely, the rebound resilience is sacrificed when a large amount of fillers are added to improve the strength, so that the compression set rate is increased, the relaxation of sealing stress is accelerated, and the long-term sealing effect is influenced. In addition, impurities such as proteins in the liquid medicine are easily adsorbed on the surface, dirt accumulation is caused, and pollution risks exist. Therefore, the invention prepares the medical silica gel sealing ring material with excellent thermal-oxidative aging resistance and antifouling property. Disclosure of Invention The invention aims to provide a medical silica gel sealing ring material and a preparation method thereof, which are used for solving the problems in the prior art. In order to solve the technical problems, the invention provides the following technical scheme: a medical silica gel sealing ring material is prepared by uniformly mixing and reacting modified silica gel, modified mica powder and grafts. Preferably, the modified silica gel is obtained by reacting vinyl silicone oil, thioglycerol and methacryloyl ethyl sulfobetaine. Preferably, the vinyl silicone oil is 100000cps from Shenzhen Xinwangsheng New Material Co. The modified mica powder is obtained by uniformly mixing and reacting mica powder, phytic acid, diglycidyl ether and allyl glycidyl ether. Preferably, the mica powder is 325 mesh in size and comes from a tourmaline mineral product processing factory in Lingshou county. Preferably, the grafts are prepared by reacting 4- (2-aminoethyl) phenylboronic acid with 3,3' -dihydroxy- [1,1' -biphenyl ] -4,4' -dicarboxaldehyde. The preparation method of the medical silica gel sealing ring material comprises the following preparation steps: (1) Uniformly mixing mica powder, phytic acid, diglycidyl ether, allyl glycidyl ether and deionized water according to the mass ratio of 1 (0.4-0.6) (0.1-0.2) (0.05-0.07) (25-35), carrying out ultrasonic treatment at 55-65 ℃ for 23-25 hours, centrifuging, washing with deionized water for 3-5 times, and drying at 55-65 ℃ for 11-13 hours to obtain modified mica powder; (2) 4- (2-amino ethyl) phenylboric acid, 3' -dihydroxyl- [1,1' -biphenyl ] -4,4' -dicarboxaldehyde, a 3A molecular sieve and absolute ethyl alcohol according to the mass ratio of 1: (0.7-0.8): (0.2-0.3): (15-25) mixing uniformly, stirring at 20-30 ℃ and 100-300 rpm for 25-35 min, taking out a molecular sieve, carrying out vacuum filtration, adding a phosphoric acid solution with the mass fraction of 80% -90% which is 5-15 times that of 4- (2-amino ethyl) phenylboronic acid, heating to 65-75 ℃ and refluxing for 2-4 h, adding deionized water with the mass of 70-80 times that of 4- (2-amino ethyl) phenylboronic acid, adding sodium bicarbonate to adjust the pH value to 8-9, continuing stirring for 25-35 min, adding ethyl acetate extraction liquid with the mass of 70-80 times that of 4- (2-amino ethyl) phenylboronic acid, adding organic phase into sodium sulfate for drying, adding ethyl oxalate solution with the mass of 70-80 times that of 4- (2-amino ethyl) phenylboronic acid, standing and precipitating, then filtering, adding deionized water with the mass of 70-80 times that of 4- (2-amino ethyl) phenylboronic acid, continuously adjusting the pH value to 8-9, stirring for 25-35 min, adding ethyl bicarbonate into the ethyl acetate ext