CN114395816A - Ultralow-elongation oil-free polypropylene short fiber for epidemic prevention mask and preparation method thereof - Google Patents
Ultralow-elongation oil-free polypropylene short fiber for epidemic prevention mask and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask and a preparation method thereof, and relates to the technical field of chemical fibers. When the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is prepared, trihydrazinobenzene, p-bromophenol and 3-epoxyethyl-3-bromopropylene are mixed to generate porous polycarbazole, and the modified polypropylene fiber with high crosslinking density is prepared; then, under the illumination condition, depositing the mixed gas of aniline and carbon dioxide on the modified polypropylene fiber, generating a large number of oxazolidone molecular chains in the pore canal of the modified polypropylene fiber, and forming a micro-nano structure containing oleophobic oxazolidone on the surface of the modified polypropylene fiber to prepare the ultralow-elongation oil-free polypropylene short fiber for the anti-epidemic mask; the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask, which is prepared by the invention, has lower elongation and good waterproof, oleophobic and antibacterial properties.
Description
Technical Field
The invention relates to the technical field of chemical fibers, in particular to an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask and a preparation method thereof.
Background
From 2019 to the present, the occurrence of epidemic situation has great influence on the economic development and social stability of countries in the world. Meanwhile, the rhythm and stability of the daily life of people are greatly influenced. In the period, the epidemic prevention mask plays an important role, and can effectively reduce the contact of people and germs, thereby preventing the spread of epidemic situations. Therefore, the epidemic prevention mask also becomes an indispensable product in daily life of people, and the epidemic prevention mask has the characteristic of non-secondary use, so that the market demand of the epidemic prevention mask is very large.
In recent years, the attention and requirements of people on the field of epidemic prevention masks are increasing due to the repetition of epidemic situations, people want the epidemic prevention masks to have good antibacterial property, waterproof property, high adsorbability, difficult deformation and the like, and the polypropylene short fibers serving as the raw materials of the epidemic prevention masks are required to have the antibacterial property, the waterproof property, the low elongation and the like, so that the technical problem to be broken through in the field of manufacturing the polypropylene short fibers is also provided.
The invention focuses on the current situation, and solves the problem by preparing the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask.
Disclosure of Invention
The invention aims to provide an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is characterized in that the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is prepared by depositing mixed gas of aniline and carbon dioxide on modified polypropylene fiber under the illumination condition.
Furthermore, the modified polypropylene fiber is obtained by mixing trihydrazinobenzene, p-bromophenol and 3-epoxy ethyl-3-bromopropylene.
Further, the preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask comprises the following preparation steps:
(1) mixing 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing sodium sulfite with ethanol, and then adjusting the pH value with sulfuric acid to prepare a sodium bisulfite solution; refluxing the mixed solution, a potassium hydroxide solution, tetrabutylammonium bromide and tetrahydrofuran in a mixed oil bath, then dropwise adding a 3-epoxyethyl-3-bromopropylene solution, sequentially extracting with dichloromethane and water, and performing rotary evaporation to prepare a spinning solution; putting the spinning solution into a spinning box, spinning by using a screw extruder, and cooling and solidifying by cross air blowing to prepare modified polypropylene fibers;
(2) mixing aniline gasified at high temperature and high pressure with carbon dioxide gas to prepare mixed gas; and (3) putting the modified polypropylene fiber into a closed container, introducing mixed gas, pressurizing and heating, depositing under the illumination condition, taking out, washing and drying to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask.
Further, the preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask comprises the following preparation steps:
(1) putting the spinning solution into a 189-190 ℃ spinning box, spinning by using a screw extruder with a 0.2-0.3 mm aperture spinneret plate under the conditions of 230-260 ℃ and 600-800 m/min spinning speed, and carrying out side-blowing cooling and curing for 30-40 min under the conditions of 14-20 ℃, 25-30% of humidity and 0.8-1.5 m/s of wind speed to prepare the modified polypropylene fiber;
(2) putting the modified polypropylene fiber into a closed container, vacuumizing for 30-40 min at 10-20 Pa, introducing mixed gas with the mass being 8-9 times that of the modified polypropylene fiber at 30-50 mL/min, pressurizing to 2.4-2.6 MPa at 30-40 Pa/min, heating to 138-142 ℃ at 2-4 ℃/min, illuminating for 13-15 h, taking out, washing for 1-3 times with deionized water, putting into a 50-60 ℃ oven, drying for 1.3-1.7 h, and cutting into 3-4 cm short fibers by using a cutting machine to obtain the ultralow-elongation oilless polypropylene short fibers for the epidemic prevention mask.
Further, the preparation method of the spinning solution in the step (1) comprises the following steps: mixing the mixed solution, 10-12% by mass of potassium hydroxide solution, tetrabutylammonium bromide and tetrahydrofuran in a mass ratio of 1: 0.9: 0.9: 49-1: 1: 0.11: 50, putting the mixture into an oil bath kettle at 70-72 ℃, stirring and refluxing for 25-35 min at 1200-1300 r/min, then dropwise adding a 3-epoxyethyl-3-bromopropylene solution with the mass being 2-3 times of that of the mixed solution at 40-60 drops/min, continuously refluxing for 9.8-10.2 h, sequentially extracting for 2-4 times by using dichloromethane and water, and then carrying out rotary evaporation for 1-2 h at 1200-1400 r/min at 50-60 ℃ under 10-20 Pa to prepare the spinning solution.
Further, the preparation method of the 3-epoxy ethyl-3-bromopropylene solution comprises the following steps: at the temperature of 24-26 ℃, mixing 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether according to the mass ratio of 1: 0.4: 10-1: 0.6: 12, stirring for 30-40 min at a speed of 1200-1300 r/min to prepare the 3-epoxy ethyl-3-bromopropylene solution.
Further, the preparation method of the mixed solution comprises the following steps: trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15-1: 16, mixing, putting into an oil bath kettle at 35-45 ℃, stirring and refluxing for 1-2 hours at 1200-1300 r/min, heating to 130-132 ℃ at 2-4 ℃, then dropwise adding a sodium bisulfite solution with the mass of 0.8-1.2 times of that of trihydrazinobenzene at 80-100 drops/min, stirring for 15-25 minutes at 1200-1300 r/min, dropwise adding p-bromophenol with the mass of 3-4 times of that of trihydrazinobenzene at 80-100 drops/min, continuously stirring and refluxing for 23-25 hours, dropwise adding a potassium hydroxide solution with the mass fraction of 10-12% at 40-60 drops/min to adjust the pH to 6.8-7.2, and then steaming for 30-40 minutes at 1200-1400 r/min at 10-20 Pa and 35-45 ℃ to prepare the mixed solution.
Further, the preparation method of the sodium bisulfite solution is as follows: at the temperature of 24-26 ℃, mixing sodium sulfite and ethanol according to the mass ratio of 1: 4-1: 6, stirring for 30-40 min at 1200-1300 r/min, then dropwise adding a sulfuric acid solution with the mass fraction of 10-12% at 40-60 drops/min to adjust the pH value to 3-4, and continuously stirring for 30-40 min to prepare the sodium bisulfite solution.
Further, the preparation method of the mixed gas in the step (2) is as follows: putting aniline into a reaction kettle at 185-187 ℃ and 0.3-0.5 MPa, preserving the temperature for 3-4 h, and introducing carbon dioxide with the mass of 2.2-2.4 times of that of the aniline at 3-5 m/s to prepare mixed gas.
Further, the illumination intensity of the illumination in the step (2) is 550-750 lx.
Compared with the prior art, the invention has the following beneficial effects:
when the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is prepared, trihydrazinobenzene, p-bromophenol and 3-epoxyethyl-3-bromopropylene are mixed to prepare the modified polypropylene fiber; and then, depositing the mixed gas of aniline and carbon dioxide on the modified polypropylene fiber under the illumination condition to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask.
Firstly, trihydrazinobenzene, p-bromophenol and 3-epoxy ethyl-3-bromopropylene are mixed to prepare modified polypropylene fibers, the hydrazine in the trihydrazinobenzene and the phenol in the p-bromophenol are subjected to a Boolean reaction to generate tricarbazole, and debromination in the tricarbazole is performed to generate porous polycarbazole, so that the porosity and the adsorbability of the modified polypropylene fibers are enhanced; bromine atoms of part of the 3-epoxy ethyl-3-bromopropylene and imino on the tricarbazole are substituted, the 3-epoxy ethyl-3-bromopropylene is firmly grafted on the porous polycarbazole, propylene in the other part of the 3-epoxy ethyl-3-bromopropylene is polymerized to form polypropylene, the polypropylene reacts with the propylene on the porous polycarbazole to form covalent bond crosslinking, the epoxy ethyl is exposed on the surface of the modified polypropylene fiber and the surface of a pore channel, and the crosslinking density of the modified polypropylene fiber is enhanced, so that the elongation of the modified polypropylene fiber is reduced.
Secondly, depositing the mixed gas of aniline and carbon dioxide on the modified polypropylene fibers under the illumination condition to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask, wherein part of the carbon dioxide and the aniline are quickly adsorbed by the modified polypropylene fibers and are fully filled in the pore channels of the modified polypropylene fibers, and react with epoxy groups on the surface of the pore channels under the photocatalysis of porous polycarbazole to generate a large number of oxazolidone molecular chains in the pore channels, so that the steric hindrance is formed in the pore channels, pathogenic bacteria can be effectively blocked, captured and killed, and the antibacterial property of the polypropylene short fiber is enhanced; and the other part of carbon dioxide and aniline are deposited on the pore-free part of the surface of the modified polypropylene fiber and react with the surface epoxy group under the photocatalysis of porous polycarbazole to generate oleophobic oxazolidinone, and meanwhile, a micro-nano structure is formed on the surface of the modified polypropylene fiber, so that the water resistance and the oil resistance of the polypropylene short fiber are enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are provided to illustrate the method in detail, and the method for testing each index of the ultra-low elongation oil-free polypropylene staple fiber for anti-epidemic mask prepared in the following examples is as follows:
and (3) antibacterial property: the antibacterial rate of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask prepared by the same mass of the embodiment and the comparative example is tested according to the GB/T20944.3 standard method.
Water resistance: the epidemic prevention mask prepared by the same mass of the embodiment and the comparative example is tested for water resistance by testing a contact angle with the ultra-low elongation oil-free polypropylene short fiber according to a GB/T4745 standard method.
Oleophobic property: the anti-epidemic masks prepared by the same mass of the examples and the comparative examples are subjected to oil repellency measurement by using the ultra-low elongation oil-free polypropylene short fiber according to the oil resistance grade of the AATCC118 standard test.
Elongation percentage: the ultra-low elongation oil-free polypropylene short fiber for the epidemic prevention mask prepared by the same length of the example and the comparative example is used for measuring the elongation at break according to the ISO3060 standard.
Example 1
A preparation method of an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask comprises the following preparation steps:
(1) at the temperature of 24 ℃, mixing sodium sulfite and ethanol according to the mass ratio of 1: 4, mixing, stirring at 1200r/min for 30min, then dripping sulfuric acid solution with the mass fraction of 10% at 40 drops/min to adjust the pH value to 3, and continuously stirring for 30min to prepare sodium bisulfite solution; trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15 mixing, putting into a 35 ℃ oil bath, stirring and refluxing for 1h at 1200r/min, heating to 130 ℃ at 2 ℃, then dropwise adding a sodium bisulfite solution with the mass of 0.8 time of the trihydrazinobenzene at 80 drops/min, stirring for 15min at 1200r/min, dropwise adding p-bromophenol with the mass of 3 times of the trihydrazinobenzene at 80 drops/min, continuously stirring and refluxing for 23h, dropwise adding a potassium hydroxide solution with the mass fraction of 10% at 40 drops/min to adjust the pH to 6.8, and then rotatably steaming for 30min at 1200r/min at 10Pa and 35 ℃ to prepare a mixed solution; at the temperature of 24 ℃, 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether are mixed according to the mass ratio of 1: 0.4: 10, stirring for 30min at 1200r/min to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 10, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 0.9: 0.9: 49 mixing, putting into a 70 ℃ oil bath, stirring and refluxing for 25min at 1200r/min, then dropwise adding a 3-epoxy ethyl-3-bromopropylene solution with the mass 2 times that of the mixed solution at 40 drops/min, continuously refluxing for 9.8h, sequentially extracting for 2 times by using dichloromethane and water, and then rotatably steaming for 1h at 1200r/min at 10Pa and 50 ℃ to prepare a spinning solution; putting the spinning solution into a 189 ℃ spinning box, spinning by using a screw extruder with a 0.2mm aperture spinneret plate under the conditions of 230 ℃ and 600m/min spinning speed, and carrying out side-blowing cooling and curing for 30min under the conditions of 14 ℃, 25% humidity and 0.8m/s wind speed to prepare the modified polypropylene fiber;
(2) placing aniline into a reaction kettle at 185 ℃ and 0.3MPa, preserving heat for 3 hours, and introducing carbon dioxide with the mass of 2.2 times that of the aniline at 3m/s to prepare mixed gas; putting the modified polypropylene fiber into a closed container, vacuumizing for 30min at 10Pa, introducing mixed gas with the mass 8 times that of the modified polypropylene fiber at 30mL/min, pressurizing to 2.4MPa at 30Pa/min, heating to 138 ℃ at 2 ℃/min, illuminating for 13h at 550lx illumination, taking out, washing for 1 time by deionized water, putting into a 50 ℃ oven for drying for 1.3h, and cutting into 3cm short fibers by a cutting machine to obtain the ultralow-elongation oil-free polypropylene short fibers for the epidemic prevention mask.
Example 2
A preparation method of an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask comprises the following preparation steps:
(1) at 25 ℃, mixing sodium sulfite and ethanol according to a mass ratio of 1: 5, mixing, stirring at 1250r/min for 35min, then dropwise adding a sulfuric acid solution with the mass fraction of 11% at 50 drops/min to adjust the pH value to 3.5, and continuously stirring for 35min to prepare a sodium bisulfite solution; trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15.5, placing the mixture into a 40 ℃ oil bath, stirring and refluxing for 1.5h at 1250r/min, heating to 131 ℃ at 3 ℃, then dropwise adding a sodium bisulfite solution 1 time of the mass of trihydrazinobenzene at 90 drops/min, stirring for 20min at 1250r/min, dropwise adding p-bromophenol 3.5 times of the mass of trihydrazinobenzene at 90 drops/min, continuously stirring and refluxing for 24h, dropwise adding a potassium hydroxide solution with the mass fraction of 11% at 50 drops/min to adjust the pH to 7, and then carrying out rotary evaporation for 35min at 1300r/min at 15Pa and 40 ℃ to prepare a mixed solution; at 25 ℃, 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether are mixed according to the mass ratio of 1: 0.5: 11, stirring at 1250r/min for 35min to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 11%, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 0.95: 1: 49.5, placing the mixture into an oil bath kettle at 71 ℃, stirring and refluxing for 30min at 1250r/min, then dropwise adding a 3-epoxy ethyl-3-bromopropylene solution with the mass 2.5 times of that of the mixed solution at 50 drops/min, continuously refluxing for 10h, sequentially extracting for 3 times by using dichloromethane and water, and then carrying out rotary evaporation for 1.5h at 1300r/min at 15Pa and 55 ℃ to prepare a spinning solution; putting the spinning solution into a 189.5 ℃ spinning box, spinning by using a screw extruder with a 0.25mm aperture spinneret plate under the conditions of 245 ℃ and 700m/min spinning speed, and carrying out side-blowing cooling and curing for 35min under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed to prepare the modified polypropylene fiber;
(2) placing aniline into a reaction kettle at 186 ℃ and 0.4MPa, preserving heat for 3.5h, and introducing carbon dioxide with the mass of 2.3 times that of the aniline at 4m/s to prepare mixed gas; putting the modified polypropylene fiber into a closed container, vacuumizing for 35min at 15Pa, introducing mixed gas with the mass 8.5 times of that of the modified polypropylene fiber at 40mL/min, pressurizing to 2.5MPa at 35Pa/min, heating to 140 ℃ at 3 ℃/min, illuminating for 14h at 600lx illumination, taking out, washing for 2 times with deionized water, putting into an oven at 55 ℃ for drying for 1.5h, and cutting into short fibers of 3.5cm by a cutting machine to prepare the ultralow-elongation oil-free polypropylene short fibers for the epidemic prevention mask.
Example 3
A preparation method of an ultralow-elongation oil-free polypropylene short fiber for an epidemic prevention mask comprises the following preparation steps:
(1) at 26 ℃, mixing sodium sulfite and ethanol according to a mass ratio of 1: 6, mixing, stirring for 40min at 1300r/min, then dropwise adding a 12% sulfuric acid solution at 60 drops/min to adjust the pH value to 4, and continuously stirring for 40min to prepare a sodium bisulfite solution; trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 16, mixing, putting into a 45 ℃ oil bath, stirring and refluxing for 2h at 1300r/min, heating to 132 ℃ at 4 ℃, then dropwise adding a sodium bisulfite solution 1.2 times of the mass of trihydrazinobenzene at 100 drops/min, stirring for 25min at 1300r/min, dropwise adding p-bromophenol 4 times of the mass of trihydrazinobenzene at 100 drops/min, continuously stirring and refluxing for 25h, dropwise adding a potassium hydroxide solution with the mass fraction of 12% at 60 drops/min to adjust the pH to 7.2, and then carrying out rotary evaporation for 40min at 1400r/min at 20Pa and 45 ℃ to prepare a mixed solution; at 26 ℃, mixing 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether according to a mass ratio of 1: 0.6: 12, stirring at 1300r/min for 40min to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 12%, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 1: 0.11: mixing 50 parts of the raw materials, putting the mixture into a 72 ℃ oil bath, stirring and refluxing for 35min at 1300r/min, then dropwise adding a 3-epoxy ethyl-3-bromopropylene solution with the mass being 3 times that of the mixed solution at 60 drops/min, continuously refluxing for 10.2h, sequentially extracting for 4 times by using dichloromethane and water, and then carrying out rotary evaporation for 2h at 1400r/min at 20Pa and 60 ℃ to prepare a spinning solution; putting the spinning solution into a spinning box at 190 ℃, spinning by using a screw extruder with a spinneret plate with the aperture of 0.3mm under the conditions of 260 ℃ and 800m/min of spinning speed, and carrying out side-blowing cooling and curing for 40min under the conditions of 20 ℃, 30% of humidity and 1.5m/s of wind speed to prepare the modified polypropylene fiber;
(2) placing aniline into a reaction kettle at 187 ℃ and 0.5MPa, preserving heat for 4 hours, and introducing carbon dioxide with the mass of 2.4 times that of the aniline at 5m/s to prepare mixed gas; putting the modified polypropylene fiber into a closed container, vacuumizing for 40min at 20Pa, introducing mixed gas with the mass 9 times that of the modified polypropylene fiber at 50mL/min, pressurizing to 2.6MPa at 40Pa/min, heating to 142 ℃ at 4 ℃/min, illuminating for 15h at 750lx illumination, taking out, washing for 3 times by deionized water, putting into a 60 ℃ oven for drying for 1.7h, and cutting into 4cm short fibers by a cutting machine to obtain the ultralow-elongation oil-free polypropylene short fibers for the epidemic prevention mask.
Comparative example 1
Comparative example 1 differs from example 2 only in step (1), step (1) being modified: at 25 ℃, mixing sodium sulfite and ethanol according to a mass ratio of 1: 5, mixing, stirring at 1250r/min for 35min, then dropwise adding a sulfuric acid solution with the mass fraction of 11% at 50 drops/min to adjust the pH value to 3.5, and continuously stirring for 35min to prepare a sodium bisulfite solution; trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15.5, placing the mixture into a 40 ℃ oil bath, stirring and refluxing for 1.5h at 1250r/min, heating to 131 ℃ at 3 ℃, then dropwise adding a sodium bisulfite solution 1 time of the mass of trihydrazinobenzene at 90 drops/min, stirring for 20min at 1250r/min, dropwise adding p-bromophenol 3.5 times of the mass of trihydrazinobenzene at 90 drops/min, continuously stirring and refluxing for 24h, dropwise adding a potassium hydroxide solution with the mass fraction of 11% at 50 drops/min to adjust the pH to 7, and then carrying out rotary evaporation for 35min at 1300r/min at 15Pa and 40 ℃ to prepare a mixed solution; at 25 ℃, mixing propylene, lauroyl peroxide and diethyl ether in a mass ratio of 1: 0.5: 11, mixing, and stirring at 1250r/min for 35min to prepare a propylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 11%, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 0.95: 1: 49.5, placing the mixture into an oil bath kettle at 71 ℃, stirring and refluxing for 30min at 1250r/min, then dropwise adding a propylene solution with the mass 2.5 times that of the mixed solution at 50 drops/min, continuously refluxing for 10h, sequentially extracting for 3 times by using dichloromethane and water, and then carrying out rotary evaporation at 1300r/min for 1.5h at 15Pa and 55 ℃ to prepare a spinning solution; and (3) putting the spinning solution into a 189.5 ℃ spinning box, spinning by using a screw extruder with a 0.25mm pore diameter spinneret plate under the conditions of 245 ℃ and 700m/min spinning speed, and carrying out side-blowing cooling and curing for 35min under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed to prepare the modified polypropylene fiber. The rest of the preparation steps are the same as example 2.
Comparative example 2
Comparative example 2 differs from example 2 only in step (1), step (1) being modified: at 25 ℃, mixing sodium sulfite and ethanol according to a mass ratio of 1: 5, mixing, stirring at 1250r/min for 35min, then dropwise adding a sulfuric acid solution with the mass fraction of 11% at 50 drops/min to adjust the pH value to 3.5, and continuously stirring for 35min to prepare a sodium bisulfite solution; trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15.5 mixing, putting into a 40 ℃ oil bath pot, stirring and refluxing for 1.5h at 1250r/min, heating to 131 ℃ at 3 ℃, then dropwise adding a sodium bisulfite solution with the mass of 1 time of trihydrazinobenzene at 90 drops/min, stirring and refluxing for 24h at 1250r/min, dropwise adding a potassium hydroxide solution with the mass fraction of 11% at 50 drops/min to adjust the pH to 7, and then carrying out rotary evaporation for 35min at 1300r/min at 15Pa and 40 ℃ to prepare a mixed solution; at 25 ℃, 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether are mixed according to the mass ratio of 1: 0.5: 11, stirring at 1250r/min for 35min to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 11%, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 0.95: 1: 49.5, placing the mixture into an oil bath kettle at 71 ℃, stirring and refluxing for 30min at 1250r/min, then dropwise adding a 3-epoxy ethyl-3-bromopropylene solution with the mass 2.5 times of that of the mixed solution at 50 drops/min, continuously refluxing for 10h, sequentially extracting for 3 times by using dichloromethane and water, and then carrying out rotary evaporation for 1.5h at 1300r/min at 15Pa and 55 ℃ to prepare a spinning solution; and (3) putting the spinning solution into a 189.5 ℃ spinning box, spinning by using a screw extruder with a 0.25mm pore diameter spinneret plate under the conditions of 245 ℃ and 700m/min spinning speed, and carrying out side-blowing cooling and curing for 35min under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed to prepare the modified polypropylene fiber. The rest of the preparation steps are the same as example 2.
Comparative example 3
Comparative example 2 differs from example 2 only in step (1), step (1) being modified: at 25 ℃, mixing sodium sulfite and ethanol according to a mass ratio of 1: 5, mixing, stirring at 1250r/min for 35min, then dropwise adding a sulfuric acid solution with the mass fraction of 11% at 50 drops/min to adjust the pH value to 3.5, and continuously stirring for 35min to prepare a sodium bisulfite solution; p-bromophenol and ethanol are mixed according to a mass ratio of 1: 15.5 mixing, putting into a 40 ℃ oil bath, stirring and refluxing for 1.5h at 1250r/min, heating to 131 ℃ at 3 ℃, then dropwise adding a sodium bisulfite solution with the mass 1 time of that of p-bromophenol at 90 drops/min, stirring and refluxing for 24h at 1250r/min, dropwise adding a potassium hydroxide solution with the mass fraction of 11% at 50 drops/min to adjust the pH to 7, and then carrying out rotary evaporation for 35min at 1300r/min at 15Pa and 40 ℃ to prepare a mixed solution; at 25 ℃, 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether are mixed according to the mass ratio of 1: 0.5: 11, stirring at 1250r/min for 35min to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing the mixed solution, a potassium hydroxide solution with the mass fraction of 11%, tetrabutylammonium bromide and tetrahydrofuran according to the mass ratio of 1: 0.95: 1: 49.5, placing the mixture into an oil bath kettle at 71 ℃, stirring and refluxing for 30min at 1250r/min, then dropwise adding a 3-epoxy ethyl-3-bromopropylene solution with the mass 2.5 times of that of the mixed solution at 50 drops/min, continuously refluxing for 10h, sequentially extracting for 3 times by using dichloromethane and water, and then carrying out rotary evaporation for 1.5h at 1300r/min at 15Pa and 55 ℃ to prepare a spinning solution; and (3) putting the spinning solution into a 189.5 ℃ spinning box, spinning by using a screw extruder with a 0.25mm pore diameter spinneret plate under the conditions of 245 ℃ and 700m/min spinning speed, and carrying out side-blowing cooling and curing for 35min under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed to prepare the modified polypropylene fiber. The rest of the preparation steps are the same as example 2.
Comparative example 4
Comparative example 4 differs from example 2 only in step (2), step (2) being modified: placing aniline into a reaction kettle at 186 ℃ and 0.4MPa, preserving heat for 3.5h, and introducing carbon dioxide with the mass of 2.3 times that of the aniline at 4m/s to prepare mixed gas; putting the modified polypropylene fiber into a closed container, vacuumizing for 35min at 15Pa, introducing mixed gas with the mass 8.5 times of that of the modified polypropylene fiber at 40mL/min, pressurizing to 2.5MPa at 35Pa/min, heating to 140 ℃ at 3 ℃/min, carrying out heat preservation reaction for 14h, taking out, washing for 2 times by using deionized water, putting into a 55 ℃ oven, drying for 1.5h, and cutting into 3.5cm short fibers by using a cutting machine to obtain the ultralow-elongation oil-free polypropylene short fibers for the epidemic prevention mask. The rest of the preparation steps are the same as example 2.
Comparative example 5
Comparative example 5 differs from example 2 only in step (2), step (2) being modified: placing aniline into a reaction kettle at 186 ℃ and 0.4MPa, and preserving heat for 3.5 hours to prepare gaseous aniline; putting the modified polypropylene fiber into a closed container, vacuumizing for 35min at 15Pa, introducing gaseous aniline with the mass 8.5 times of that of the modified polypropylene fiber at 40mL/min, pressurizing to 2.5MPa at 35Pa/min, heating to 140 ℃ at 3 ℃/min, illuminating for 14h at 600lx illumination, taking out, washing for 2 times with deionized water, putting into an oven at 55 ℃ for drying for 1.5h, and cutting into 3.5cm short fibers by a cutting machine to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask. The rest of the preparation steps are the same as example 2.
Comparative example 6
Comparative example 6 differs from example 2 only in step (2), step (2) being modified: putting the modified polypropylene fiber into a closed container, vacuumizing for 35min at 15Pa, introducing carbon dioxide with the mass 8.5 times of that of the modified polypropylene fiber at 40mL/min, pressurizing to 2.5MPa at 35Pa/min, heating to 140 ℃ at 3 ℃/min, illuminating for 14h at 600lx illumination, taking out, washing for 2 times with deionized water, putting into an oven at 55 ℃ for drying for 1.5h, and cutting into 3.5cm short fibers by a cutting machine to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask. The rest of the preparation steps are the same as example 2.
Examples of effects
Table 1 below shows the results of the analysis of the elongation, water and oil repellency, and antibacterial property of the ultra-low elongation oil-free polypropylene staple fiber for an anti-epidemic mask prepared in examples 1 to 3 and comparative examples 1 to 6 of the present invention.
TABLE 1
From table 1, it can be seen that the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask prepared in examples 1, 2 and 3 has relatively low elongation and good water and oil repellency and antibacterial property; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 1, it can be found that when propylene is used for preparing the modified polypropylene fiber, the cross-linking density of the modified polypropylene fiber is low, and subsequently, when aniline and carbon dioxide mixed gas is used for depositing on the modified polypropylene fiber under the illumination condition, oxazolidinone cannot be formed, so that the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask has high elongation and weak oleophobicity and antibacterial property; from the experimental data of examples 1, 2 and 3 and comparative examples 2 and 3, it can be found that porous polycarbazole cannot be formed when the modified polypropylene fiber is prepared without using trihydrazinobenzene or p-bromophenol, the crosslinking density of the modified polypropylene fiber is low, and oxazolidinone and a micro-nano structure cannot be formed when the modified polypropylene fiber is deposited with a mixed gas of aniline and carbon dioxide under the illumination condition, so that the ultra-low-elongation oil-free polypropylene short fiber for the epidemic prevention mask has high elongation and low water, oil and microbial resistance; from the experimental data of examples 1, 2, 3 and comparative example 4, it can be found that, when the mixed gas of aniline and carbon dioxide is deposited on the modified polypropylene fiber without illumination, oxazolidinone and micro-nano structure can not be formed, so that the water and oil repellency and the antibacterial property are weak; from the experimental data of examples 1, 2, 3 and comparative example 5, it can be found that, under the illumination condition, the modified polypropylene fiber deposited by using gaseous aniline cannot form oxazolidinone, so that the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask has weaker oleophobicity and antibacterial property; from the experimental data of examples 1, 2, 3 and comparative example 6, it can be seen that, under the illumination condition, the modified polypropylene fiber deposited by carbon dioxide can not form oxazolidone, and lipophilic cyclic carbonate is generated, so that the ultra-low elongation oil-free polypropylene short fiber for the epidemic prevention mask has weak oil repellency, weak antibacterial property and strong waterproof property.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is characterized in that the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask is prepared by depositing mixed gas of aniline and carbon dioxide on modified polypropylene fiber under the illumination condition.
2. The method for preparing the ultra-low elongation oil-free polypropylene staple fiber for the epidemic prevention mask as claimed in claim 1, wherein the modified polypropylene fiber is obtained by mixing trihydrazinobenzene, p-bromophenol and 3-epoxyethyl-3-bromopropylene.
3. The preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask according to claim 1, wherein the preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask comprises the following preparation steps:
(1) mixing 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether to prepare a 3-epoxy ethyl-3-bromopropylene solution; mixing sodium sulfite with ethanol, and then adjusting the pH value with sulfuric acid to prepare a sodium bisulfite solution; refluxing the mixed solution, a potassium hydroxide solution, tetrabutylammonium bromide and tetrahydrofuran in a mixed oil bath, then dropwise adding a 3-epoxyethyl-3-bromopropylene solution, sequentially extracting with dichloromethane and water, and performing rotary evaporation to prepare a spinning solution; putting the spinning solution into a spinning box, spinning by using a screw extruder, and cooling and solidifying by cross air blowing to prepare modified polypropylene fibers;
(2) mixing aniline gasified at high temperature and high pressure with carbon dioxide gas to prepare mixed gas; and (3) putting the modified polypropylene fiber into a closed container, introducing mixed gas, pressurizing and heating, depositing under the illumination condition, taking out, washing and drying to prepare the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask.
4. The preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask according to claim 3, wherein the preparation method of the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask comprises the following preparation steps:
(1) putting the spinning solution into a 189-190 ℃ spinning box, spinning by using a screw extruder with a 0.2-0.3 mm aperture spinneret plate under the conditions of 230-260 ℃ and 600-800 m/min spinning speed, and carrying out side-blowing cooling and curing for 30-40 min under the conditions of 14-20 ℃, 25-30% of humidity and 0.8-1.5 m/s of wind speed to prepare the modified polypropylene fiber;
(2) putting the modified polypropylene fiber into a closed container, vacuumizing for 30-40 min at 10-20 Pa, introducing mixed gas with the mass being 8-9 times that of the modified polypropylene fiber at 30-50 mL/min, pressurizing to 2.4-2.6 MPa at 30-40 Pa/min, heating to 138-142 ℃ at 2-4 ℃/min, illuminating for 13-15 h, taking out, washing for 1-3 times with deionized water, putting into a 50-60 ℃ oven, drying for 1.3-1.7 h, and cutting into 3-4 cm short fibers by using a cutting machine to obtain the ultralow-elongation oilless polypropylene short fibers for the epidemic prevention mask.
5. The method for preparing the ultra-low elongation oil-free polypropylene staple fiber for the epidemic prevention mask according to claim 4, wherein the preparation method of the spinning solution in the step (1) is as follows: mixing the mixed solution, 10-12% by mass of potassium hydroxide solution, tetrabutylammonium bromide and tetrahydrofuran in a mass ratio of 1: 0.9: 0.9: 49-1: 1: 0.11: 50, putting the mixture into an oil bath kettle at 70-72 ℃, stirring and refluxing for 25-35 min at 1200-1300 r/min, then dropwise adding a 3-epoxyethyl-3-bromopropylene solution with the mass being 2-3 times of that of the mixed solution at 40-60 drops/min, continuously refluxing for 9.8-10.2 h, sequentially extracting for 2-4 times by using dichloromethane and water, and then carrying out rotary evaporation for 1-2 h at 1200-1400 r/min at 50-60 ℃ under 10-20 Pa to prepare the spinning solution.
6. The method for preparing the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask according to claim 5, wherein the preparation method of the 3-epoxyethyl-3-bromopropylene solution comprises the following steps: at the temperature of 24-26 ℃, mixing 3-epoxy ethyl-3-bromopropylene, lauroyl peroxide and diethyl ether according to the mass ratio of 1: 0.4: 10-1: 0.6: 12, stirring for 30-40 min at a speed of 1200-1300 r/min to prepare the 3-epoxy ethyl-3-bromopropylene solution.
7. The method for preparing the ultra-low elongation oil-free polypropylene staple fiber for the epidemic prevention mask according to claim 5, wherein the preparation method of the mixed solution is as follows: trihydrazinobenzene and ethanol are mixed according to a mass ratio of 1: 15-1: 16, mixing, putting into an oil bath kettle at 35-45 ℃, stirring and refluxing for 1-2 hours at 1200-1300 r/min, heating to 130-132 ℃ at 2-4 ℃, then dropwise adding a sodium bisulfite solution with the mass of 0.8-1.2 times of that of trihydrazinobenzene at 80-100 drops/min, stirring for 15-25 minutes at 1200-1300 r/min, dropwise adding p-bromophenol with the mass of 3-4 times of that of trihydrazinobenzene at 80-100 drops/min, continuously stirring and refluxing for 23-25 hours, dropwise adding a potassium hydroxide solution with the mass fraction of 10-12% at 40-60 drops/min to adjust the pH to 6.8-7.2, and then steaming for 30-40 minutes at 1200-1400 r/min at 10-20 Pa and 35-45 ℃ to prepare the mixed solution.
8. The method for preparing the ultralow-elongation oil-free polypropylene short fiber for the epidemic prevention mask according to claim 7, wherein the method for preparing the sodium bisulfite solution comprises the following steps: at the temperature of 24-26 ℃, mixing sodium sulfite and ethanol according to the mass ratio of 1: 4-1: 6, stirring for 30-40 min at 1200-1300 r/min, then dropwise adding a sulfuric acid solution with the mass fraction of 10-12% at 40-60 drops/min to adjust the pH value to 3-4, and continuously stirring for 30-40 min to prepare the sodium bisulfite solution.
9. The method for preparing the ultra-low elongation oil-free polypropylene staple fiber for the epidemic prevention mask according to claim 4, wherein the method for preparing the mixed gas in the step (2) is as follows: putting aniline into a reaction kettle at 185-187 ℃ and 0.3-0.5 MPa, preserving the temperature for 3-4 h, and introducing carbon dioxide with the mass of 2.2-2.4 times of that of the aniline at 3-5 m/s to prepare mixed gas.
10. The method for preparing the ultra-low elongation oil-free polypropylene staple fiber for the epidemic prevention mask according to claim 4, wherein the illumination intensity of the illumination in the step (2) is 550 to 750 lx.
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