Silicone fibers and methods for making the same
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SUZHOU UNIV
- Filing Date
- 2025-06-05
- Publication Date
- 2026-05-12
AI Technical Summary
而现有的报道采用的PDMS预聚物,主体是聚二甲基硅氧烷,即使交联后也会存在交联密度低和分布较窄的情况;且聚二甲基硅氧烷侧链甲基(-CH3)的存在会削弱分子间作用力从而造成分子链缠结下降、拉伸强度降低
[0031]This invention involves compounding terminal vinyl silicone oil, side vinyl silicone oil, and hydrogen-based silicone oil in a specific ratio to obtain a ternary silicone oil spinning solution, and then preparing organosilicon fibers using a high-temperature air-induced crosslinking and curing method. Compared to oil bath heating, which may generate harmful gases, this method uses air heating, making it non-toxic and environmentally friendly. Furthermore, this method is simple to prepare, significantly shortens the processing cycle, and allows for continuous production.
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Figure CN120649193B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of organosilicon materials technology, and more specifically, relates to an organosilicon fiber and its preparation method. Background Technology
[0002] Organosilicon materials possess the advantage of high-temperature resistance, making them a preferred material for many new technologies. Their fabrication into flexible and easily processed fibers offers even wider applications. However, due to their inherent characteristics, organosilicon materials are difficult to spin using traditional melt spinning and solution spinning methods. But cross-linking in the presence of a catalyst provides a potential approach for the fiberization of organosilicon materials. Currently, there are relatively few strategies for cross-linking spinning of organosilicon materials. Most preparation strategies rely on template methods and oil bath curing methods, which not only result in high production costs and complex processes, hindering industrialization, but also lead to uneven fiber thickness produced by the oil bath method, significantly affecting the fiber's mechanical properties. Surveys have found that existing organosilicon fibers all use polydimethylsiloxane (PDMS) and corresponding curing agents as raw materials, resulting in generally low tensile strength, which is insufficient to meet practical application requirements.
[0003] The following are some of the problems with existing technologies:
[0004] Existing technologies include the preparation of silicone fibers using PDMS prepolymer and curing agent as raw materials, mixed and heated in an oil bath. Fibers prepared by this method exhibit irregular cross-sections and uneven thickness due to the buoyancy of the oil bath during curing, resulting in poor luster and tensile strength ranging from 2.7 to 9.2 MPa. Furthermore, the curing oil bath used in this experiment releases small amounts of toxic gases at high temperatures. Alternatively, PDMS prepolymer and curing agent are mixed, injected into a mold for curing, and then ejected to obtain silicone fibers. While this mold method allows for controlled circular cross-sections, it is costly, complex, and typically produces short fibers in a single operation; the tensile strength of the resulting fibers falls far short of practical requirements. Another method uses coaxial wet spinning of PDMS prepolymer and curing agent to prepare helical fibers, but this also suffers from insufficient tensile strength.
[0005] Organosilicon fibers are cross-linked polymers, and the degree of cross-linking within them significantly impacts their mechanical properties. Existing reports utilize PDMS prepolymers, primarily polydimethylsiloxane, which, even after cross-linking, exhibit low cross-linking density and narrow distribution. Furthermore, the presence of methyl groups (-CH3) on the side chains of polydimethylsiloxane weakens intermolecular forces, leading to reduced molecular chain entanglement and lower tensile strength. In addition, while both mold-based and oil-bath methods have partially filled the gaps in organosilicon fiber preparation, they suffer from low production efficiency and uneven fiber cross-sections. This causes stress concentration in the thinner sections of the fiber under tensile stress, leading to breakage. Therefore, producing organosilicon fibers with high tensile properties remains a challenge. Summary of the Invention
[0006] The purpose of this invention is to address the above-mentioned shortcomings by providing an organosilicon fiber and its preparation method. The method uses air heating of liquid silicone oil active components, and traction stretching during the cross-linking and curing reaction of the active components, thereby efficiently spinning organosilicon fibers. The core technical problem solved is to ensure that the silicone oil active components are stable and fluid at room temperature, and that they can be rapidly cured under air heating conditions with an adjustable curing rate, thereby ensuring complete curing and shaping during the traction stretching process to form fibers.
[0007] To achieve the above objectives, the present invention is implemented through the following technical solution:
[0008] In a first aspect, the present invention provides an organosilicon fiber, wherein the raw materials of the organosilicon fiber include a silicone oil spinning solution and additives, wherein the silicone oil spinning solution includes vinyl silicone oil and hydrogen-based silicone oil in a mass ratio of 1:(0.8~1.4), wherein the vinyl silicone oil includes terminal vinyl silicone oil and side vinyl silicone oil, and the amount of side vinyl silicone oil added is 0~20wt%; the additives include a catalyst, an inhibitor and a coordination dissociation agent, each added in an amount of 0.1 wt%~1 wt% of the silicone oil spinning solution content.
[0009] Preferably, the mass ratio of the vinyl silicone oil to the hydrogen-based silicone oil is 1:(1.1~1.2), and the amount of side vinyl silicone oil added to the vinyl silicone oil is 14 wt%~16 wt%.
[0010] Preferably, the vinyl-terminated silicone oil is a divinyl-terminated phenyl silicone oil with a viscosity of 500 cp to 3000 cp and a vinyl content of 0.8% to 1.2%; it includes one or more of α,ω-vinyl polymethylphenylsiloxane, α,ω-vinyl poly(methylphenylsiloxane-dimethylsiloxane), or α,ω-vinyl poly(dimethylsiloxane-diphenylsiloxane); preferably α,ω-vinyl polymethylphenylsiloxane with a viscosity of 950 to 1050 cp and a vinyl content of 0.8% to 1.2%; its structural formula is as follows:
[0011] ;
[0012] Where n is 30~300.
[0013] Preferably, the side-vinyl silicone oil is an end-sided polyvinylphenyl silicone oil with a viscosity of 500 cp to 10000 cp and a vinyl content of 2.3% to 2.7%; it includes one or more of α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) or α,ω-vinyl poly(phenylvinylsiloxane-methylphenylsiloxane); preferably α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) with a viscosity of 5000 cp and a vinyl content of 2.3% to 2.7%; its structural formula is as follows:
[0014] ;
[0015] Where m is 50~500; n is 5~50.
[0016] Preferably, the hydrogen-based silicone oil is a side-containing hydrogen silicone oil, comprising α,ω-dimethylpolymethylhydrosiloxane, with a viscosity of 80 cp to 100 cp, and a hydrogen content of 0.36% to 1.6%; its structural formula is as follows:
[0017] ;
[0018] Where n is between 20 and 100.
[0019] Preferably, the additive further includes a filler, which is hydrophobic fumed silica, and the mass ratio of the filler to the spinning solution is 1:(5~99).
[0020] Preferably, the catalyst is a platinum catalyst, including any one of Speier catalyst and Karstedt catalyst, and the platinum concentration in the platinum catalyst is 1000 ppm to 10000 ppm; preferably, a Karstedt catalyst is used, with the following structural formula:
[0021] .
[0022] Preferably, the inhibitor is any one of acetylenol, 2-methyl-3-butanol-2-ol, or butynediol, and the inhibitor concentration is 1000 ppm to 10000 ppm; wherein, the structural formula of acetylenol is [insert structural formula here]. The structural formula of 2-methyl-3-butanol-2-ol is: The structural formula of butynediol is: .
[0023] Preferably, the coordination dissociation agent is a borate ester, including methyl borate, ethyl borate, butyl borate, or pinacol diborate, and the concentration of the coordination dissociation agent is 1000 ppm to 10000 ppm; wherein, the structural formula of methyl borate is [insert structural formula here]. The structural formula of ethyl borate is: The structural formula of butyl borate is: The structural formula of pinacol diboronate is: .
[0024] In a second aspect, the present invention provides a method for preparing the organosilicon fiber described in the first aspect, comprising:
[0025] Vinyl silicone oil and hydrogen-based silicone oil are mixed evenly in a certain proportion to prepare a silicone oil spinning solution;
[0026] Inhibitor, catalyst and coordination dissociation agent were added sequentially to the obtained silicone oil spinning solution and stirred to obtain spinning solution prepolymer.
[0027] The above-mentioned spinning solution prepolymer is added to the spinning equipment, and cross-linking and curing are induced by air heating, and then spun into fibers.
[0028] Preferably, the silicone oil spinning solution is prepared at a temperature of 0℃~50℃ and a stirring rate of 100~1000rpm; the temperature for heating-induced crosslinking and curing is 100℃~250℃.
[0029] Preferably, the spinning equipment includes a constant pressure injection pump, a spinning head and a heat insulation support, a heating sleeve, a temperature control device, and a collection device. The spinning solution prepolymer is propelled into the spinning head by the constant pressure injection pump and output to the collection device through the spinning head to solidify. The heating sleeve is fitted over the spinning head. The temperature control device is used to adjust the temperature of the heating sleeve so that the spinning solution is stretched and pulled while being induced to crosslink and solidify in situ by air heating when passing through the spinning head.
[0030] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0031] This invention involves compounding terminal vinyl silicone oil, side vinyl silicone oil, and hydrogen-based silicone oil in a specific ratio to obtain a ternary silicone oil spinning solution, and then preparing organosilicon fibers using a high-temperature air-induced crosslinking and curing method. Compared to oil bath heating, which may generate harmful gases, this method uses air heating, making it non-toxic and environmentally friendly. Furthermore, this method is simple to prepare, significantly shortens the processing cycle, and allows for continuous production.
[0032] This invention uses air-heated liquid silicone oil active components, and pulls and stretches them during the cross-linking and curing reaction of the active components, thereby spinning organosilicon fibers with high efficiency. The core technical problem solved is to ensure that the silicone oil active components are stable and fluid at room temperature, and that they can be rapidly cured under air heating conditions with an adjustable curing rate, so as to ensure complete curing and shaping during the traction and stretching process to form fibers.
[0033] This invention regulates the degree of internal crosslinking of the produced organosilicon fibers by adjusting the ratio of end vinyl silicone oil, side vinyl silicone oil and hydrogen-based silicone oil in the ternary spinning solution, thereby obtaining organosilicon fibers with excellent mechanical properties such as elasticity and strength. This opens up applications for organosilicon materials beyond silicone oil, silicone rubber and silicone resin, giving organosilicon materials a wider range of applications.
[0034] This invention adds a coordination dissociation agent, borate ester, which can esterify with the alkynol inhibitor in the component under high temperature conditions, thereby further dissociating the inhibitor-platinum coordination and rapidly releasing the platinum catalyst. This achieves rapid curing, ensuring complete curing during the fiber spinning traction process and avoiding defects such as dripping and fiber deformation during spinning.
[0035] The organosilicon fibers prepared by this invention exhibit excellent heat resistance, waterproof and breathable properties, and good biocompatibility. Combined with the advantages of organosilicon fibers being woven and spun, these fibers can be used as specialty fibers and textiles. For example, organosilicon fibers can be woven into waterproof fabrics for outdoor protective applications such as tents, as well as for umbrellas and raincoats. Due to their high-temperature resistance, organosilicon fibers can be used to prepare high-temperature protective clothing fabrics or fabric-based high-temperature resistant composite materials, and as thermochromic fabrics for signal indication in high-temperature environments. Organosilicon fibers can also be used as medical textiles that come into direct contact with the human body. Because organosilicon fibers possess excellent elasticity, blending them with other fibers can produce apparel or industrial textiles with excellent mechanical properties such as elasticity. Attached Figure Description
[0036] Figure 1 This is a schematic diagram illustrating the crosslinking reaction principle for preparing organosilicon fibers according to the present invention.
[0037] Figure 2 A schematic diagram of the spinning process of silicone fibers using the silicone fiber spinning apparatus provided in this embodiment of the invention;
[0038] Figure 3 The images show the ultra-depth-of-field three-dimensional microscope and SEM images of the organosilicon fibers prepared in Example 1; where (a1) and (a2) are the cross-sectional SEM morphology of SiF@H1, (a3) is the morphology of the cross-section of SiF@H1 under ultra-depth-of-field three-dimensional microscope, (b1) and (b2) are the longitudinal surface SEM morphology of SiF@H1, and (b3) is the morphology of the longitudinal surface of SiF@H1 under ultra-depth-of-field three-dimensional microscope.
[0039] Figure 4 The image shows the surface elemental distribution of the organosilicon fiber prepared in Example 1; where (a) and (b) are the elemental distributions of the cross section and longitudinal surface of SiF@H1, respectively.
[0040] Figure 5 Tensile properties of organosilicon fibers prepared from hydrogen-based silicone oils with different hydrogen contents;
[0041] Figure 6 The diagram shows the effect of end-side vinyl silicone oil on the performance of silicone fibers. (a) shows the effect of viscosity and addition amount of end-side polyvinylphenyl silicone oil on the tensile properties of silicone fibers; (b) shows the schematic diagram of lifting different weight hooks on the silicone fiber SiF@H1-15 (5000) prepared in Example 2.
[0042] Figure 7 The fatigue resistance test diagrams of the organosilicon fiber SiF@H1-15 (5000) prepared in Example 2 are shown in (a) and (b) are the stress-strain curves of SiF@H1-15 (5000) after the first 5 cycles of cyclic tensile testing.
[0043] Figure 8 Electron micrograph of the organosilicon fiber prepared in Comparative Example 7.
[0044] In the diagram: 1. Constant pressure injection pump; 2. Spinning head and heat insulation bracket; 3. Heating sleeve; 4. Temperature control device; 5. Collection device. Detailed Implementation
[0045] Existing spinning methods mainly employ the die method and the oil bath curing method. The die method involves injecting the mixed spinning solution into a tube of another material, followed by heating and curing. This method typically produces coarse fibers, with short fiber lengths produced in a single operation. Furthermore, due to the difficulty of cleaning the die interior, it is generally only used once, resulting in high costs. The oil bath method utilizes the instantaneous curing of the spinning solution upon contact with a high-temperature oil bath, which to some extent overcomes the limitations of the die method. However, it also presents several problems: (a) As a fluid, the spinning solution is subject to buoyancy upon contact with the oil bath. Due to variations in the contact surface mass, the cured fibers will ultimately exhibit a spindle shape, accompanied by uneven fiber thickness. (b) While increasing the oil bath temperature has some effect in accelerating the curing of the spinning solution, temperatures above 200°C decompose the oil, producing harmful gases and deteriorating the working environment. (c) The contamination of the fibers by the oil bath during contact with the spinning solution and the formed fibers is also significant. Therefore, a more efficient, non-toxic, and low-cost spinning method is needed.
[0046] Excluding the complex operations of the mold method, using a high-temperature heat source to heat and solidify the silicone spinning solution is a better way to achieve rapid fiber forming. To avoid the impact of oil bath curing on fiber morphology, this invention designs a high-temperature air-induced cross-linking and curing method. A temperature-controlled annular heating sleeve is designed. When the temperature of the heating sleeve increases, the temperature of the surrounding air also rises rapidly. At this time, when the silicone spinning solution passes through the center of the heating sleeve at a certain rate, it is rapidly heated, solidified, and cross-linked. During this process, it is stretched and drawn to form fiber materials with controllable cross-section and diameter. The fiber cross-section prepared in this way can be regularly circular and uniform in thickness. This spinning process does not involve heating with other liquid media and involves almost no emission of harmful gases.
[0047] The method for preparing organosilicon fibers provided by this invention is as follows: (1) preparation of silicone oil spinning solution; (2) prepolymerization; (3) high-temperature air-induced crosslinking and curing into fibers. The specific steps are as follows:
[0048] S1: Preparation of silicone oil spinning solution:
[0049] Add the terminal vinyl silicone oil, side vinyl silicone oil, and hydrogen-based silicone oil to a container in a certain proportion and stir until fully mixed.
[0050] S2: Prepolymerization:
[0051] The silicone oil spinning solution mixed evenly in S1 was placed in a constant temperature water bath, and the inhibitor, catalyst and coordination dissociation agent were added dropwise in sequence. The mixture was stirred at a certain rate to prepolymerize the spinning solution to a spinnable state.
[0052] S3: High-temperature air-induced cross-linking and curing into filaments:
[0053] The spinning solution prepolymer obtained in S2 above is poured into a spinning device, and then cross-linked and cured into filaments by high-temperature air-induced cross-linking to obtain organosilicon fibers. The cross-linking reaction in this process is as follows: Figure 1 As shown.
[0054] In the above reaction process, the presence of the inhibitor can block the platinum catalyst, thereby slowing down the rate of the hydrosilylation reaction and providing a longer shelf life, allowing the spinning solution to be stored for an extended period. Adjusting the temperature of the spinning equipment to instantly raise the temperature of the spinning solution releases the catalyst, which then re-catalyzes the hydrosilylation reaction, allowing the spinning solution to solidify into fibers in a short time. Simultaneously, due to the addition of borate ester coordination dissociators, these esters undergo transesterification with the inhibitor at high temperatures, rapidly dissociating the inhibitor from the platinum coordination structure and releasing the platinum catalyst to catalyze the hydrosilylation crosslinking reaction. The reaction equation for the dynamic equilibrium reached between the alkynol inhibitor, the catalyst, and the borate ester coordination dissociator under high-temperature conditions through transesterification and coordination reactions is as follows:
[0055] .
[0056] Preferred embodiments of the present invention will now be described in more detail with reference to the accompanying drawings and specific examples.
[0057] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, and the materials and reagents used are commercially available.
[0058] The raw materials used in the specific embodiments are as follows:
[0059] Vinyl-terminated silicone oil: α,ω-vinyl polymethylphenylsiloxane, 1000cp, Guoyan Chemical New Materials Co., Ltd.;
[0060] Side-bound vinyl silicone oil: α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane), 5000 cp, Guoyan Chemical New Materials Co., Ltd.;
[0061] Hydrogen-based silicone oil: α,ω-dimethyl polymethylhydrosiloxane, hydrogen content 0.75%, Shenzhen Jipeng Silicon Fluorine Materials Co., Ltd.;
[0062] Inhibitor: Weigh 0.05 g of butynediol (Shanghai Aladdin Biochemical Technology Co., Ltd.) and add isopropanol, then dilute to 10 mL with a volumetric flask to prepare a solution with an alkynediol concentration of 5000 ppm.
[0063] Coordination dissociation agent: Weigh 0.05 g of dipinaol ester of borate (Shanghai Aladdin Biochemical Technology Co., Ltd.), add isopropanol, and dilute to 10 mL with a volumetric flask to prepare a solution of borate ester coordination dissociation agent with a concentration of 5000 ppm;
[0064] Catalyst: Karstedt catalyst, platinum content 3000 ppm, Shenzhen Kejunchi Industrial Co., Ltd.
[0065] The measurement methods in the following embodiments include:
[0066] (1) The mechanical properties of the prepared silicone fibers were tested using an INSTRON-3365 dual-arm material testing machine. According to the national standard GB / T 14337-2022 for testing the tensile properties of short chemical fibers, the fibers were cut to a length of 4 cm and both ends were wrapped with labels. The sensor used in the test had a range of 0~8 N, and the tensile speed was 4 cm·min. -1 The spacing was 2 cm. To ensure more accurate measurements, each fiber sample was tested an average of 20 times to obtain the average tensile strength and elongation at break. Furthermore, keeping the fiber stretching rate constant, the fiber was subjected to 150 cycles of cyclic stretching at 100% elongation to study the fatigue resistance of SiF.
[0067] (2) Linear density is one of the most important indicators for characterizing fiber thickness. Commonly used units are tex (Nt), decitex (Ndt), and denier (ND). Measure and cut a length of silicon fiber, accurately weigh the fiber on an electronic balance, and then calculate the linear density of the silicone fiber using the following formula:
[0068] ;
[0069] Where: L is the length of the fiber (m), and m is the mass of the fiber (g).
[0070] (3) The crosslinking density of fibers with different amounts of vinyl silicone oil added can be tested using the toluene swelling method. First, a section of fiber is cut and weighed, and then soaked in toluene solution for 72 hours to ensure sufficient swelling. After 72 hours, the fiber is removed, the surface of the fiber is wiped dry with filter paper, and then weighed immediately. The formula for calculating the crosslinking density is as follows:
[0071] ;
[0072] ;
[0073] Where: ρ1 is the fiber density (g·mL) -1 ), ρ2 is the density of toluene (g·mL) -1 w1 and w2 are the masses (g) before and after swelling, v e v0 is the crosslinking density and v0 is the molar volume of toluene.
[0074] Example 1:
[0075] This embodiment provides an organosilicon fiber, the preparation method of which includes the following steps:
[0076] S1: Preparation of silicone oil spinning solution
[0077] Take a clean container and add 37.8 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp) and 2.2 g of α,ω-dimethyl polymethylhydrosiloxane (0.75% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm to obtain silicone oil spinning solution.
[0078] S2: Prepolymer
[0079] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0080] S3: High-temperature air-induced cross-linking and curing into filaments
[0081] The spinning solution prepolymer is added to the spinning equipment after being fully degassed. The spinning equipment used in this embodiment is as follows: Figure 2 As shown, the device includes a constant pressure injection pump 1, a spinning head and heat insulation support 2, a heating sleeve 3, a temperature control device 4, and a collection device 5. The spinning process involves the spinning solution prepolymer being propelled into the spinning head by the constant pressure injection pump 1, and then output to the collection device 5 through the spinning head to solidify. The heating sleeve 3 is fitted over the spinning head, and the temperature control device 4 is used to adjust the temperature of the heating sleeve 3 so that the spinning solution prepolymer is stretched and pulled while being induced to crosslink and solidify in situ by air heating when passing through the spinning head.
[0082] Specifically, after fully degassing the spinning solution prepolymer prepared in S2, it is injected into a 50 mL syringe, which is then clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 is set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. When the spinning solution prepolymer passes through the heating sleeve at a uniform speed, it is stretched and tractioned while simultaneously undergoing in-situ cross-linking and curing. It is then completely cured and formed upon entering the rotating collection cage, resulting in an organosilicon fiber product, designated SiF@H1.
[0083] The morphology and structure of the organosilicon fiber SiF@H1 prepared in this embodiment are as follows: Figure 3 As shown, from Figure 3As can be seen, the cross-section of the organosilicon fiber is a regular circle with smooth longitudinal direction; the surface elemental distribution of SiF@H1 is as follows: Figure 4 As shown in the figure, the silicone fiber is composed of three elements: Si, O, and C. The diameter of the fiber was measured at 10 different points on the same fiber, and the average diameter of the silicone fiber SiF@H1 was calculated to be 300 ± 13 μm. The tensile strength of SiF@H1 was measured to be 0.65 cN·tex using a dual-arm material testing machine. -1 The elongation at break was 518.47%.
[0084] Comparative Example 1:
[0085] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0086] S1: Preparation of silicone oil spinning solution
[0087] Take a clean container and add 35.6 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp) and 4.4 g of α,ω-dimethyl polymethylhydrosiloxane (0.36% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm to obtain silicone oil spinning solution.
[0088] S2: Prepolymer
[0089] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0090] S3: High-temperature air-induced cross-linking and curing into filaments
[0091] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. When the spinning solution passed through the heating sleeve at a uniform speed, it underwent stretching and in-situ cross-linking and curing simultaneously, and was fully cured upon entering the rotating collection cage, resulting in an organosilicon fiber product, designated SiF@H0. The tensile strength of SiF@H0 was measured to be 0.24 cN·tex using a double-arm material testing machine. -1 The elongation at break was 616.19%.
[0092] Comparative Example 2:
[0093] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0094] S1: Preparation of silicone oil spinning solution
[0095] Take a clean container and add 38.3g of α,ω-vinyl polymethylphenylsiloxane (1000 cp) and 1.7g of α,ω-dimethyl polymethylhydrosiloxane (1.0% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm to obtain the silicone oil spinning solution.
[0096] S2: Prepolymer
[0097] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0098] S3: High-temperature air-induced cross-linking and curing into filaments
[0099] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. When the spinning solution passed through the heating sleeve at a uniform speed, it underwent stretching and in-situ cross-linking and curing simultaneously, and was fully cured upon entering the rotating collection cage, resulting in an organosilicon fiber product, designated SiF@H2. The tensile strength of SiF@H2 was measured to be 0.53 cN·tex using a double-arm material testing machine. -1 The elongation at break was 489.54%.
[0100] Comparative Example 3:
[0101] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0102] S1: Preparation of silicone oil spinning solution
[0103] Take a clean container and add 39.0 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp) and 4.4 g of α,ω-dimethyl polymethylhydrosiloxane (1.6% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm to obtain silicone oil spinning solution.
[0104] S2: Prepolymer
[0105] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0106] S3: High-temperature air-induced cross-linking and curing into filaments
[0107] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. When the spinning solution passed through the heating sleeve at a uniform speed, it underwent stretching and in-situ cross-linking and curing simultaneously, and was fully cured upon entering the rotating collection cage, resulting in an organosilicon fiber product, designated SiF@H3. The tensile strength of SiF@H3 was measured to be 0.15 cN·tex using a double-arm material testing machine. -1 The elongation at break was 334.46%.
[0108] The effect of hydrogen content in hydrogen-based silicone oil on the mechanical properties of organosilicon fibers was analyzed using Examples 1, 1, 2, and 3.
[0109] The hydrogen content of hydrogen-based silicone oil reflects the number of active sites that can undergo hydrosilylation with -CH=CH2. Therefore, this application systematically studies the effect of the hydrogen content of hydrogen-based silicone oil on the mechanical properties of fibers. Figure 5 The tensile properties of organosilicon fibers prepared from hydrogen-based silicone oils with different hydrogen contents are shown in the figure. As shown, when the hydrogen content of the hydrogen-based silicone oil is 0.36%, the tensile strength of the prepared SiF@H0 is relatively low, only about 0.24 cN·tex. -1However, the elongation at break is very high, reaching over 600%. With increasing hydrogen content, the tensile strength of the fiber initially increases and then decreases. This is because when the hydrogen content is low (0.36%), only a few crosslinks occur within SiF@H0. At this point, when a load is applied to both ends of the fiber, the internal macromolecules are not bound and can freely orient and extend, resulting in high elongation. The limited number of crosslinking points means fewer load-bearing molecular chains per unit area, leading to very low tensile strength and limited application value. When the hydrogen content in the hydrogen-containing silicone oil increases to 0.75%, the crosslinking points move closer together, the crosslinking density increases, and there are more crosslinking nodes per unit area bearing external stress, thus increasing the fiber strength. The strength of SiF@H1 reaches 0.65 cN·tex. -1 However, when the hydrogen content of silicone oil is too high, the crosslinking points become too dense, leading to a shortened distance between crosslinked chains. This reduces the uniformity of crosslinking point distribution, resulting in locally overly dense crosslinking. When subjected to external force, fewer molecular chains share the stress. In this situation, the fiber's molecular chains are easily damaged by stress concentration, resulting in a decrease in tensile strength (e.g., SiF@H2 and SiF@H3). Conversely, the elongation at break of the fiber decreases with increasing hydrogen content in the hydrogen-based silicone oil.
[0110] Example 2: Effect of the amount and viscosity of the side-vinyl silicone oil on mechanical properties
[0111] This embodiment provides an organosilicon fiber, the preparation method of which includes the following steps:
[0112] S1: Preparation of silicone oil spinning solution
[0113] Take a clean container and add 32.5 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp), 4.8 g of α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) (5000 cp), and 2.6 g of α,ω-dimethyl polymethylhydrosiloxane (0.75% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm.
[0114] S2: Prepolymer
[0115] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0116] S3: High-temperature air-induced cross-linking and curing into filaments
[0117] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. The resulting silicone fiber product was designated SiF@H1-15(5000). The tensile strength of SiF@H1-15(5000) was measured to be 1.14 cN·tex using a double-arm material testing machine. -1 With a breaking elongation of 248.50%, a single fiber can easily lift a 150g hook weight, such as... Figure 6 As shown; in addition, SiF@H1-15 also has excellent cyclic tensile properties, maintaining good mechanical properties after 150 cycles of stretching at 100% elongation, such as... Figure 7 As shown.
[0118] Example 3: Effect of the amount of side-vinyl silicone oil added on the mechanical properties of organosilicon fibers
[0119] This embodiment provides an organosilicon fiber. Except for the amounts of α,ω-vinyl polymethylphenylsiloxane (1000 cp) (35.7 g) and α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) (5000 cp) (1.6 g), the other component ratios and preparation methods are the same as in Example 2. The resulting organosilicon fiber product is designated SiF@H1-5(5000). The tensile strength of SiF@H1-5(5000) was measured to be 0.77 cN·tex using a double-arm material testing machine. -1 The elongation at break is 375.17%.
[0120] Example 4: Effect of the amount of side-vinyl silicone oil added on the mechanical properties of organosilicon fibers
[0121] This embodiment provides an organosilicon fiber. Except for the amounts of α,ω-vinyl polymethylphenylsiloxane (1000 cp) (33.1 g) and α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) (5000 cp) (3.2 g), the amounts of other components and the preparation method are the same as in Example 2. The resulting organosilicon fiber product is designated SiF@H1-10(5000). The tensile strength of SiF@H1-10(5000) was measured to be 1.07 cN·tex using a double-arm material testing machine. -1 The elongation at break was 317.12%.
[0122] Comparative Example 4: Effect of the viscosity of vinyl ester silicone oil on the mechanical properties of silicone fibers
[0123] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0124] S1: Preparation of silicone oil spinning solution
[0125] Take a clean container and add 32.5 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp), 4.8 g of α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) (500 cp), and 2.6 g of α,ω-dimethyl polymethylhydrosiloxane (0.75% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm.
[0126] S2: Prepolymer
[0127] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0128] S3: High-temperature air-induced cross-linking and curing into filaments
[0129] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. The obtained silicone fiber product was designated SiF@H1-15(500). The tensile strength of SiF@H1-15(500) was measured to be 0.47 cN·tex using a double-arm material testing machine. -1 The elongation at break was 428.87%.
[0130] Comparative Example 5: Effect of the viscosity of vinyl silicone oil on the mechanical properties of silicone fibers
[0131] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0132] S1: Preparation of silicone oil spinning solution
[0133] Take a clean container and add 32.5 g of α,ω-vinyl polymethylphenylsiloxane (1000 cp), 4.8 g of α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) (1000 cp), and 2.6 g of α,ω-dimethyl polymethylhydrosiloxane (0.75% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm.
[0134] S2: Prepolymer
[0135] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor butylene glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt and 0.1% of dipinacol diboron ester were added. The system temperature was controlled at 25°C, and the mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0136] S3: High-temperature air-induced cross-linking and curing into filaments
[0137] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃. The resulting silicone fiber product was designated SiF@H1-15(1000). The tensile strength of SiF@H1-15(1000) was measured to be 0.55 cN·tex using a double-arm material testing machine. -1 The elongation at break was 361.78%.
[0138] The effects of viscosity and addition amount of end-sided vinyl silicone oil on the mechanical properties of silicone fibers were analyzed through Examples 1, 2, 3, 4, Comparative Example 4, and Comparative Example 5.
[0139] While changing the hydrogen content of hydrogen-based silicone oil can improve the tensile strength of silicon fibers to some extent, the effect on strength improvement is limited due to the small molecular weight and low crosslinking point distribution of end vinyl silicone oil. Therefore, introducing side vinyl silicone oil can further improve the mechanical properties of fibers and has achieved significant results. Figure 6(a) Comparison of the mechanical properties of fibers with different viscosities and addition amounts of side vinyl silicone oil. The figure shows that the silicone fibers without side vinyl silicone oil have lower strength and higher elongation at break. However, after adding 5 wt%, 10 wt%, and 15 wt% side vinyl silicone oil (5000 cp) respectively, the tensile strength gradually increases, reaching 0.77 cN·tex. -1 1.07 cN·tex -1 and 1.14 cN·tex -1 The mechanical properties of SiF@H1-15 (5000) are optimal. This is because the addition of side vinyl silicone oil allows for more cross-linking within the fiber molecules. Calculations show that the degrees of cross-linking for SiF@H1, SiF@H1-5 (5000), SiF@H1-10 (5000), and SiF@H1-15 (5000) are 0.15, 0.30, 0.42, and 0.68, respectively, consistent with theoretical analysis. Under tension, the fiber macromolecules initially undergo moderate elongation of the molecular chain segments to adapt to the external force. However, due to the limitation of cross-linking, the fiber molecules collectively bear the external force after elongating to a certain extent, thus increasing the strength. When the amount of side vinyl silicone oil exceeds 15 wt%, a phenomenon of difficulty in rapid curing occurs during spinning, which may be due to the structure of the side vinyl silicone oil. Compared to end-vinyl silicone oils, the vinyl and phenyl groups in side-vinyl silicone oils are close to each other. As is well known, the phenyl group is a sterically hindered group, which will prevent the reaction between Si-CH=CH2 and Si-H, making it difficult to crosslink and form within the specified curing time.
[0140] To more intuitively demonstrate the strength of SiF@H1-15 (5000), weights of different masses were lifted from SiF@H1-15 (5000) single fibers. Figure 6 As shown in (b), SiF@H1-15 (5000) can easily lift a 150 g weight, demonstrating a significant increase in strength after blending with vinyl silicone oil. Furthermore, while the elongation at break of SiF@H1-15 (5000) decreases to approximately 250%, it still exhibits excellent elongation properties. Overall, SiF@H1-15 (5000) possesses the best mechanical properties.
[0141] The strength of fibers prepared by adding side vinyl silicone oils with viscosities of 500 cp and 1000 cp only increased slightly before starting to decrease. This may be because when the viscosity of the side vinyl silicone oil is low, the crosslinking points are more densely distributed. At this time, the movement of fiber molecular chains is restricted under the action of external force, resulting in a decrease in tensile strength.
[0142] The cyclic tensile properties of silicone fiber SiF@H1-15 (5000) are also significant in practical applications, such as... Figure 7 As shown in (a), during the overall 150 cycles of 100% tensile testing, the tensile strength of SiF@H1-15 (5000) remained essentially constant, approximately 0.13 N. The strength remained relatively good after 150 cycles. To observe the stress-strain relationship during the cyclic tensile process in more detail, Figure 7 (b) The stress-strain curves of SiF@H1-15 (5000) after the first five cycles are shown. Interestingly, the stress-strain curve of the fiber after the first stretching shows a slight lag, and the tensile strength decreases slightly under the same elongation conditions, but this phenomenon does not occur after the second cycle. Excluding slippage at both ends, we analyze the following reasons. First, under the application of external force, the fiber molecular chains continuously adjust to adapt to the external load, and in this process, they need to overcome intermolecular friction. After the first stretching, the organosilicon macromolecules rearrange and increase their order compared to the initial state, resulting in a slight decrease in strength during subsequent stretching. Furthermore, during the first stretching, some molecular chains did not rearrange their orientation in time under the action of external force and broke, which also leads to a decrease in stress after stretching. However, during 150 cycles of stretching, the mechanical properties of SiF@H1-15 (5000) remain good, exhibiting excellent fatigue resistance and meeting practical application requirements.
[0143] A comparison of the preparation methods and properties of the silicone fibers prepared in this embodiment with those of silicone fibers reported in the prior art is shown in Table 1. It can be seen that the previously reported silicone fibers were mostly prepared using mold methods and oil bath curing methods, which resulted in uneven fiber thickness and low production efficiency. Furthermore, the strength of these reported silicone fibers was generally low, limiting their application scenarios. In contrast, the SiF@H1-15 (5000) prepared in this embodiment not only has a round, uniform cross-section in appearance, but also exhibits a significant improvement in tensile strength. This is all thanks to the controllable degree of cross-linking within the fiber.
[0144] Table 1: Performance comparison of SiF@H1-15 (5000 cp) with previously reported products containing organosilicon fibers
[0145]
[0146] Note: The sources of the other reports mentioned above are as follows:
[0147] [1] Highly flexible and stretchable optical strain sensing for humanmotion detection. Optica, 2017, 4(10): 1285-1288
[0148] [2] Flexible and Optical Fiber Sensors Composited by Graphene andPDMS for Motion Detection. Polymers, 2019, 11(9):1433
[0149] [3] Sugar-plastic assisted fabrication of hollow PDMS wearablefabrics toward excellent sensory capabilities . Journal of MaterialsChemistry A, 2024, 12(12): 7237-7247
[0150] [4] Rapid mold-free fabrication of long functional PDMS fibers. NPGAsia Materials, 2022, 14(1): 13
[0151] [5] Wang Ruhai. Preparation of silicone fiber and its application in wearable devices. Master's thesis, Xi'an University of Technology, 2024.
[0152] [6] Li Lele. Preparation and application of high-performance PDMS fiber-based flexible strain sensor. Doctoral dissertation, Tianjin University, 2022.
[0153] Example 5: The effect of filler on improving the mechanical properties of organosilicon fibers
[0154] This embodiment provides an organosilicon fiber, in which 2 wt% hydrophobic fumed silica is added during the preparation of the silicone oil spinning solution. The dosage of other components and the preparation method are the same as in Example 2. The tensile strength of the filler-doped SiF@H1-15(5000)-2 is 1.08 cN·tex. -1 .
[0155] Comparative Example 6: Spinning failed without the addition of a coordination dissociator, resulting in discontinuous fibers.
[0156] This comparative example provides an organosilicon fiber, the preparation method of which includes the following steps:
[0157] S1: Preparation of silicone oil spinning solution
[0158] Take a clean container and add 37.8 g of divinyl-terminated phenyl silicone oil (1000 cp) and 2.2 g of hydrogen-based silicone oil (0.75% hydrogen content) in sequence. Mix the silicone oil evenly at a stirring speed of 500 rpm.
[0159] S2: Prepolymer
[0160] Subsequently, the above-mentioned mixed silicone oil spinning solution was placed in a constant temperature water bath, and 0.1% of the total mass of silicone oil inhibitor acetylacetonate glycol was added. The mixture was stirred for 5 min to ensure that the inhibitor was evenly distributed in the spinning solution. Then, 3000 ppm of platinum catalyst Karstedt was added, and the system temperature was controlled at 25°C. The mixture was stirred at 150 rpm for about 15 min to prepolymerize the spinning solution to a spinnable state.
[0161] S3: High-temperature air-induced cross-linking and curing into filaments
[0162] Using the spinning equipment described in Example 1, the spinning solution prepolymer prepared in S2 was fully degassed and then injected into a 50 mL syringe, which was clamped onto a constant pressure injection pump 1. The injection speed of the constant pressure injection pump 1 was set to 0.65 mL / min. -1 The actual heating temperature at the center of the heating sleeve was measured to be approximately 200℃~220℃. When the spinning solution passed through the heating sleeve at a uniform speed, the spinning solution underwent in-situ cross-linking and solidification. However, due to the high-temperature baking time of 10~60s and the absence of a coordination dissociation agent, borate ester, the platinum catalyst dissociated slowly, resulting in slow solidification. Consequently, the spun fibers broke, and spinning was unsuccessful.
[0163] Comparative Example 7: When a small amount of coordination dissociation agent is added, the cross-section of the organosilicon fiber is irregular.
[0164] This comparative example provides an organosilicon fiber. Except for the addition of dipinacol diboronate at 50% of the inhibitor mass during the prepolymerization stage, the amounts of other components and the preparation method are the same as in Comparative Example 6. The organosilicon fiber obtained by spinning has an irregular circular cross-section, as shown in the electron micrograph below. Figure 8 As shown, this is because the dissociation inhibitor is insufficient to rapidly and completely dissociate the inhibitor from the platinum ligand, resulting in a slow curing rate. This is also due to excessive stretching of the fiber before curing. Figure 8 Microfibers can also be observed on the fiber surface, which are attributed to the formation of fly filaments due to slow curing.
[0165] The various embodiments of the present invention have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and principles of the described embodiments, and these modifications and variations should also be considered within the scope of protection of the present invention.
Claims
1. An organosilicon fiber, characterized in that, The raw materials for the organosilicon fiber include silicone oil spinning solution and additives. The silicone oil spinning solution includes vinyl silicone oil and hydrogen-based silicone oil in a mass ratio of 1:(0.8~1.4). The vinyl silicone oil includes terminal vinyl silicone oil and side vinyl silicone oil, and the amount of side vinyl silicone oil added is 5 wt%~16 wt%. The additives include catalysts, inhibitors and coordination dissociation agents, each added in an amount of 0.1 wt%~1 wt% of the silicone oil spinning solution. The inhibitor is any one of ethynylcyclohexanol, 2-methyl-3-butanol-2-ol, or butynediol; the coordination dissociation agent is a borate ester.
2. The organosilicon fiber according to claim 1, characterized in that, The mass ratio of the vinyl silicone oil to the hydrogen-based silicone oil is 1:(1.1~1.2), and the amount of side vinyl silicone oil added to the vinyl silicone oil is 14 wt%~16 wt%.
3. The organosilicon fiber according to claim 1, characterized in that, The vinyl-terminated silicone oil is a divinyl-terminated phenyl silicone oil with a viscosity of 500 cp to 3000 cp and a vinyl content of 0.8% to 1.2%; it includes one or more of α,ω-vinyl polymethylphenylsiloxane, α,ω-vinyl poly(methylphenylsiloxane-dimethylsiloxane), or α,ω-vinyl poly(dimethylsiloxane-diphenylsiloxane) in any mixture.
4. The organosilicon fiber according to claim 1, characterized in that, The side-vinyl silicone oil is an end-side polyvinylphenyl silicone oil with a viscosity of 500 cp to 10000 cp and a vinyl content of 2.3% to 2.7%; it includes one or more of α,ω-vinyl poly(methylphenylsiloxane-methylvinylsiloxane) or α,ω-vinyl poly(phenylvinylsiloxane-methylphenylsiloxane) in any mixture.
5. The organosilicon fiber according to claim 1, characterized in that, The hydrogen-based silicone oil is a side-containing hydrogen silicone oil, comprising α,ω-dimethylpolymethylhydrosiloxane, with a viscosity of 80 cp to 100 cp, and a hydrogen content of 0.36% to 1.6%.
6. The organosilicon fiber according to claim 1, characterized in that, The catalyst is a platinum catalyst, which includes any one of Speier catalyst and Karstedt catalyst, and the platinum concentration in the platinum catalyst is 1000 ppm to 10000 ppm; And / or, the concentration of the inhibitor is 1000 ppm to 10000 ppm; And / or, the coordination dissociation agent includes methyl borate, ethyl borate, butyl borate or pinacol diborate, and the concentration of the coordination dissociation agent is 1000 ppm to 10000 ppm.
7. The organosilicon fiber according to claim 1, characterized in that, The additive also includes a filler, which is hydrophobic fumed silica, and the mass ratio of the filler to the spinning solution is 1:(5~99).
8. A method for preparing organosilicon fibers according to any one of claims 1 to 7, characterized in that, include: Vinyl silicone oil and hydrogen-based silicone oil are mixed evenly in a certain proportion to prepare a silicone oil spinning solution; Inhibitor, catalyst and coordination dissociation agent were added sequentially to the obtained silicone oil spinning solution and stirred to obtain spinning solution prepolymer. The above-mentioned spinning solution prepolymer is added to the spinning equipment, and cross-linking and curing are induced by air heating, and then spun into fibers.
9. The method for preparing organosilicon fibers according to claim 8, characterized in that, The silicone oil spinning solution is prepared at a temperature of 0℃~50℃. And / or, the temperature for heat-induced crosslinking curing is 60℃~250℃.
10. The method for preparing organosilicon fibers according to claim 8, characterized in that, The spinning equipment includes a constant pressure injection pump, a spinning head and heat insulation support, a heating sleeve, a temperature control device, and a collection device. The spinning solution prepolymer is propelled into the spinning head by the constant pressure injection pump and then output to the collection device through the spinning head to solidify. The heating sleeve is fitted over the spinning head. The temperature control device is used to adjust the temperature of the heating sleeve so that the spinning solution is stretched and pulled while being induced to crosslink and solidify in situ by air heating when passing through the spinning head.