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CN-122011784-A - Photo-curing type pyrimidine-terminated ketone-based silicone rubber material and preparation method thereof

CN122011784ACN 122011784 ACN122011784 ACN 122011784ACN-122011784-A

Abstract

The application discloses a photo-curing type terminal pyrimidinone silicone rubber material and a preparation method thereof, and belongs to the technical field of silicone rubber materials. The photocuring type terminal pyrimidinone silicone rubber material comprises, by weight, 100 parts of terminal pyrimidinone polysiloxane, 0-60 parts of reinforcing filler, 0.5-4 parts of cross-linking agent and 0.1-0.5 part of photoinitiator, wherein the content of siloxane in the terminal pyrimidinone polysiloxane is not less than 94wt%. The application adopts the pyrimidone-terminated polysiloxane as the rubber matrix to obviously improve the comprehensive mechanical property of the material, and cooperates with the reinforcing filler, the cross-linking agent and the photoinitiator to realize the synergistic balance of high strength, high elongation at break, low modulus and low hardness, and the comprehensive property of the prepared silicone rubber material is outstanding when the high-temperature mechanical property is obviously improved.

Inventors

  • CHENG XIAO
  • WU MANMAN
  • ZHAO YANCHENG
  • ZHOU CHUANJIAN

Assignees

  • 山东大学

Dates

Publication Date
20260512
Application Date
20260318

Claims (10)

  1. 1. The photocuring type terminal pyrimidinone silicone rubber material is characterized by comprising, by weight, 100 parts of terminal pyrimidinone polysiloxane, 0-60 parts of reinforcing filler, 0.5-4 parts of cross-linking agent and 0.1-0.5 part of photoinitiator; wherein the siloxane content in the terminal pyrimidinone-based polysiloxane is not less than 94wt%; the structural formula of the terminal pyrimidinone-based polysiloxane is shown as a formula (1): formula (1); Wherein R is one or more of methyl, phenyl and ethyl, 0<n/(m+n+p) is less than or equal to 5%, p/(m+p) is less than or equal to 0 and less than or equal to 40%, and the molecular weight is 1-60 ten thousand.
  2. 2. The photo-curable terminal pyrimidinone silicone rubber material according to claim 1, wherein the content of siloxane in the terminal pyrimidinone silicone is not less than 98wt%.
  3. 3. The photo-curable terminal pyrimidinone silicone rubber material according to claim 1, wherein the content of siloxane in the terminal pyrimidinone silicone is not less than 99wt%.
  4. 4. The photocuring type terminal pyrimidinone-based silicone rubber material according to claim 1, wherein the cross-linking agent is side chain mercaptopropyl polydimethylsiloxane, and the structural formula is shown as formula (2) or formula (3): (2), (3) Wherein, a/(a+b) is less than or equal to 10% and less than or equal to 100%.
  5. 5. The photo-curable terminated pyrimidinone based silicone rubber material according to claim 1, wherein the photo-initiator comprises one or more of 2, 2-dimethylol propionic acid, 2-dimethoxy-2-phenyl acetophenone, 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone, 1-hydroxycyclohexyl phenyl ketone, bis (2, 4, 6-trimethylbenzoyl) phenyl phosphine oxide.
  6. 6. The photo-curable terminated pyrimidinone silicone rubber material of claim 1, wherein the reinforcing filler comprises one or more of white carbon black, graphene, carbon nanotubes, gypsum fiber, carbon fiber, organoclay, boron nitride.
  7. 7. The photo-curable terminated pyrimidinone silicone rubber material according to claim 6, further comprising tea polyphenols.
  8. 8. The photo-curing type pyrimidine ketone-terminated silicone rubber material according to claim 7, wherein the amount of tea polyphenol is 0.5-3 parts by weight.
  9. 9. The method for preparing the photo-curing type pyrimidyl terminated silicone rubber material according to any one of claims 1 to 8, which is characterized by comprising the following steps: (1) Preparing raw materials according to the weight portion ratio, adding the pyrimidyl polysiloxane into an open mill, adding reinforcing filler, and uniformly mixing to obtain a rubber compound; (2) Placing the rubber compound in a double-roll open mill, adding a cross-linking agent and a photoinitiator, carrying out thin pass for several times to obtain a rubber compound, placing the rubber compound in a mould, carrying out hot press shaping in a vacuum vulcanizing machine, then carrying out ultraviolet irradiation curing, and demoulding to obtain the pyrimidyl silicone rubber material.
  10. 10. The preparation method of the photo-curing type pyrimidine ketone-terminated silicon rubber material according to claim 9, wherein the temperature of hot press setting in the step (2) is 50-180 ℃, the wavelength of ultraviolet light irradiation is 254-400 nm, and the time of ultraviolet light irradiation is 0.25-4 h.

Description

Photo-curing type pyrimidine-terminated ketone-based silicone rubber material and preparation method thereof Technical Field The application relates to a photo-curing type terminal pyrimidinone silicone rubber material and a preparation method thereof, belonging to the technical field of silicone rubber materials. Background Polysiloxane (PDMS) has excellent high and low temperature resistance, weather resistance, aging resistance, electrical insulation and biocompatibility by virtue of a unique Si-O-Si inorganic main chain structure, and is widely applied to high-end fields such as aerospace, electronic packaging, transportation, medical care and the like. However, the mechanical strength of polysiloxanes is often not satisfactory compared to carbon-based polymer rubbers. The Si-O bond has longer bond length and larger bond angle, so that the molecular chain has extremely high flexibility, and the molecular chain tends to curl into a random coil structure in a thermodynamic equilibrium state, so that the intermolecular acting force is weak, and the cohesive energy density is low. The inherent structural characteristics lead the unreinforced silicone rubber to have poorer mechanical properties, and greatly limit the application of the unreinforced silicone rubber in scenes with higher requirements on strength and toughness. Therefore, on the basis of retaining the original excellent characteristics of the silicone rubber, the mechanical strength and toughness of the silicone rubber are effectively improved, and the research is always focused in the field. The Chinese patent publication No. CN 119039787A discloses a high-strength ultraviolet curing organic silicon rubber and a preparation method thereof. The ultraviolet curing type ultraviolet curing adhesive comprises, by mass, 520 parts of hydroxyl-terminated modified silicone oil, 520 parts of alkoxy-terminated modified silicone oil, 2060 part of acryloyloxy silicone oil, 2060 part of silicone rubber reinforced prepolymer, 110 parts of acryloyloxy modified MQ silicone resin, 311 parts of white carbon black, 38 parts of polyamino organosilicon compound, 312 parts of strong reactive diluent, 312 parts of weak reactive diluent, 0.55 part of moisture curing catalyst and 0.55 part of photoinitiator. The invention solves the problem of lower strength of the organic silicon rubber to a certain extent by a multi-component synergistic and high filling reinforcement mode, but the technical scheme has obvious limitations that the preparation process is complicated. The method relies on the preparation of 'silicone rubber reinforcing prepolymer' in advance, and relates to the accurate proportioning of various silicone oils with different functional groups, the process is complex, the production efficiency is low, and the quality control difficulty is high. Therefore, developing a photo-curing silicone rubber with simple components, no complex procedure and excellent mechanical strength and toughness is a technical problem which needs to be solved at present. Disclosure of Invention In order to solve the problems, the photocuring type terminal pyrimidinone silicone rubber material and the preparation method thereof are provided, wherein the terminal pyrimidinone silicone is adopted as a rubber matrix, the comprehensive mechanical properties of the material are obviously improved, the reinforcing filler, the cross-linking agent and the photoinitiator are matched, the synergistic balance of high strength, high elongation at break, low modulus and low hardness is realized, the high-temperature mechanical properties are obviously improved, and the combination process of hot press shaping and photocuring is adopted, so that the molding efficiency is high, the process controllability is strong, and the comprehensive properties of the prepared silicone rubber material are outstanding. According to one aspect of the application, the application provides a photo-curing type terminal pyrimidinone silicone rubber material, which comprises the following raw materials, by weight, 100 parts of terminal pyrimidinone polysiloxane, 0-60 parts of reinforcing filler, 0.5-4 parts of cross-linking agent and 0.1-0.5 part of photoinitiator; wherein the siloxane content in the terminal pyrimidinone-based polysiloxane is not less than 94wt%; the structural formula of the terminal pyrimidinone-based polysiloxane is shown as a formula (1): formula (1); Wherein R is one or more of methyl, phenyl and ethyl, 0<n/(m+n+p) is less than or equal to 5%, p/(m+p) is less than or equal to 0 and less than or equal to 40%, and the molecular weight is 1-60 ten thousand. Preferably, n/(m+n+p) is 0.1% or less and 0.5% or less, and more preferably, n/(m+n+p) is 0.15% or less and 0.3% or less. Preferably, 0≤p/(m+p). Ltoreq.30%, further preferably, 0≤p/(m+p). Ltoreq.20%. Preferably, the molecular weight is 1 to 40 ten thousand, and more preferably, the molecular weight is 6 to 20 ten thousand. Specifically, the c