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CN-120649193-B - Organic silicon fiber and preparation method thereof

CN120649193BCN 120649193 BCN120649193 BCN 120649193BCN-120649193-B

Abstract

The invention discloses an organic silicon fiber and a preparation method thereof in the technical field of organic silicon materials, wherein the organic silicon fiber comprises a silicon oil spinning solution and an additive, the silicon oil spinning solution comprises vinyl silicon oil and hydrogen-based silicon oil with the mass ratio of 1 (0.8-1.4), the vinyl silicon oil comprises terminal vinyl silicon oil and side vinyl silicon oil, the addition amount of the side vinyl silicon oil in the vinyl silicon oil is 0-20wt%, and the additive comprises a catalyst, an inhibitor and a coordination dissociation agent. According to the invention, the terminal vinyl silicone oil, the side vinyl silicone oil and the hydrogen-based silicone oil are compounded in proportion to obtain the ternary silicone oil spinning solution, and then the high-temperature air induced cross-linking curing method is utilized to prepare the organic silicon fiber with excellent mechanical properties such as elasticity, strength and the like.

Inventors

  • SHI LEI
  • ZHAO MANMAN
  • GUAN JINPING
  • LI ZHANXIONG

Assignees

  • 苏州大学

Dates

Publication Date
20260512
Application Date
20250605

Claims (10)

  1. 1. The organic silicon fiber is characterized in that raw materials of the organic silicon fiber comprise a silicone oil spinning solution and an additive, wherein the silicone oil spinning solution comprises vinyl silicone oil and hydrogen-based silicone oil with the mass ratio of 1 (0.8-1.4), the vinyl silicone oil comprises terminal vinyl silicone oil and lateral vinyl silicone oil, the addition amount of the lateral vinyl silicone oil in the vinyl silicone oil is 5-wt% to 16% by weight, and the additive comprises a catalyst, an inhibitor and a coordination dissociation agent, wherein the addition amount of the catalyst, the inhibitor and the coordination dissociation agent respectively account for 0.1-wt% to 1wt% of the content of the silicone oil spinning solution; the inhibitor is any one of acetylene cyclohexanol, 2-methyl-3-butanol-2-alcohol or butynediol, and the coordination dissociation agent is boric acid esters.
  2. 2. The organic silicon fiber according to claim 1, wherein the mass ratio of the vinyl silicone oil to the hydrogen silicone oil is 1 (1.1-1.2), and the addition amount of the side vinyl silicone oil in the vinyl silicone oil is 14 wt% -16 wt%.
  3. 3. The silicone fiber of claim 1, wherein the vinyl-terminated silicone oil is a divinyl-terminated phenyl silicone oil having a viscosity of 500 cp to 3000 cp and a vinyl content of 0.8 to 1.2%, and comprises one or more of an α, ω -vinyl polymethylphenyl siloxane, an α, ω -vinyl poly (methylphenylsiloxane-dimethylsiloxane), or an α, ω -vinyl poly (dimethylsiloxane-diphenylsiloxane) in any combination.
  4. 4. The silicone fiber according to claim 1, wherein the side vinyl silicone oil is a terminal side polyvinyl phenyl silicone oil having a viscosity of 500 cp to 10000 cp and a vinyl content of 2.3 to 2.7%, and comprises one or a mixture of any of α, ω -vinyl poly (methyl phenyl siloxane-methyl vinyl siloxane) or α, ω -vinyl poly (phenyl vinyl siloxane-methyl phenyl siloxane).
  5. 5. The silicone fiber according to claim 1, wherein the hydrogen-based silicone oil is a side hydrogen-containing silicone oil, and the side hydrogen-containing silicone oil comprises alpha, omega-dimethyl polymethylhydrosiloxane, has a viscosity of 80 cp-100 cp, and has a hydrogen content of 0.36% -1.6%.
  6. 6. The silicone fiber according to claim 1, wherein, The catalyst is a platinum catalyst, the platinum catalyst comprises any one of a Speier catalyst and a Karstedt catalyst, and the platinum concentration in the platinum catalyst is 1000 ppm-10000 ppm; And/or the concentration of the inhibitor is 1000 ppm-10000 ppm; and/or the coordination and dissociation agent comprises methyl borate, ethyl borate, butyl borate or pinacol borate, and the concentration of the coordination and dissociation agent is 1000 ppm-10000 ppm.
  7. 7. The organic silicon fiber according to claim 1, wherein the additive further comprises a filler, the filler is hydrophobic fumed silica, and the mass ratio of the filler to the spinning solution is 1 (5-99).
  8. 8. A method for producing the silicone fiber according to any one of claims 1 to 7, comprising: Uniformly mixing vinyl silicone oil and hydrogen-based silicone oil according to a proportion to prepare a silicone oil spinning solution; sequentially adding an inhibitor, a catalyst and a coordination dissociation agent into the obtained silicone oil spinning solution, and stirring to obtain a spinning solution prepolymer; and adding the spinning solution prepolymer into spinning equipment, and carrying out air heating to induce crosslinking and solidification, so as to obtain the spinning solution.
  9. 9. The method for producing a silicone fiber according to claim 8, wherein, The temperature of the silicone oil spinning solution is 0-50 ℃ during preparation; and/or the temperature of the heating-induced cross-linking curing is 60-250 ℃.
  10. 10. The method for preparing the organic silicon fiber according to claim 8, wherein the spinning equipment comprises a constant pressure injection pump, a spinning head, a heat insulation support, a heating sleeve, a temperature control device and a collecting device, wherein the spinning solution prepolymer is pushed into the spinning head through the constant pressure injection pump and is output into the collecting device through the spinning head to be solidified and formed, the heating sleeve is sleeved outside the spinning head, and the temperature control device is used for adjusting the temperature of the heating sleeve, so that the spinning solution is stretched and pulled through the spinning head and is simultaneously subjected to in-situ crosslinking and solidification through air heating.

Description

Organic silicon fiber and preparation method thereof Technical Field The invention belongs to the technical field of organic silicon materials, and particularly relates to an organic silicon fiber and a preparation method thereof. Background The organosilicon material has the advantage of high temperature resistance, is the first choice material of most new technologies, and has wider application when being prepared into flexible and easily-processed fibers. However, the organosilicon material is difficult to realize traditional melt spinning and solution spinning due to the characteristics, but the cross-linking can occur in the presence of a catalyst to provide a thinking for the fiberization of the organosilicon material. At present, the strategies for crosslinking spinning of the organosilicon material are few, and most of the preparation strategies are a template method and an oil bath curing method, so that the preparation cost is high, the process is complex, industrialization is difficult to realize, and the uneven thickness of the fiber prepared by the oil bath method greatly influences the mechanical property of the fiber. It is found that the existing organic silicon fiber adopts Polydimethylsiloxane (PDMS) and corresponding curing agent as raw materials, the tensile strength of the fiber is generally low, and the actual application requirement is difficult to meet. The following are some of the problems with the prior art: In the prior art, PDMS prepolymer and curing agent are used as raw materials, and the preparation of the organic silicon fiber is realized by an oil bath heating method after mixing. The fiber prepared by the method has the advantages that the cross section is irregularly shaped, the thickness is uneven, the gloss is poor, the tensile strength of the fiber is 2.7-9.2 MPa due to the influence of the buoyancy of the oil bath when the spinning solution is solidified, and in addition, a small amount of toxic gas can be released by the solidified oil bath adopted in the experimental process at high temperature. Or PDMS prepolymer and curing agent are used as raw materials, and the raw materials are mixed, injected into a mold for curing and then ejected, so that the organosilicon fiber is obtained. The die method can manually control the cross section of the fiber to be round, but has higher cost, more complex preparation process and shorter length of the organic silicon fiber which is usually prepared at one time, and the tensile strength of the prepared fiber can not reach the actual requirement. Or the PDMS prepolymer and the curing agent are used as raw materials to prepare the spiral fiber by adopting a coaxial wet spinning method, and the prepared fiber has the problem of insufficient tensile strength. The organosilicon fiber belongs to a cross-linked polymer, and the internal cross-linking degree has an important influence on the mechanical property of the fiber. The PDMS prepolymer used in the prior report is mainly polydimethylsiloxane, even after crosslinking, the conditions of low crosslinking density and narrow distribution exist, and the existence of the methyl (-CH 3) of the side chain of the polydimethylsiloxane weakens the intermolecular acting force, so that the entanglement of molecular chains is reduced, and the tensile strength is reduced. In addition, although the die method and the oil bath method fill the gap of difficult preparation of the organosilicon fiber to a certain extent from the aspect of production technology, the methods respectively have the defects of low production efficiency and uneven fiber cross section thickness, so that stress is concentrated at the thinner part of the fiber to break when the fiber is subjected to external force stretching action, and the preparation of the organosilicon fiber with high stretching performance is still a challenge at present. Disclosure of Invention The invention aims to overcome the defects, and provides an organic silicon fiber and a preparation method thereof, wherein an air heating liquid silicone oil active component is adopted, and traction stretching is carried out in the process of crosslinking curing reaction of the active component, so that the organic silicon fiber is spun with high efficiency, the core technical problem is that the silicone oil active component is ensured to be stable and have fluidity at room temperature, is rapidly cured under the condition of air heating, and the curing rate is adjustable, so that complete curing molding in the traction stretching process is ensured, and the fiber is formed. In order to achieve the above purpose, the invention is realized by the following technical scheme: In the first aspect, the invention provides an organic silicon fiber, wherein the organic silicon fiber comprises a silicon oil spinning solution and an additive, the silicon oil spinning solution comprises vinyl silicone oil and hydrogen-based silicone oil with the mass ratio of 1 (0.8-1.4