CN109868657B - Preparation method of flame-retardant wear-resistant curtain - Google Patents
Preparation method of flame-retardant wear-resistant curtain Download PDFInfo
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Abstract
The invention discloses a preparation method of a flame-retardant wear-resistant curtain, which comprises the following specific preparation processes: grafting magnesium hydroxide in a polyurethane resin melt to obtain a loaded polyurethane polymer, mixing and refining the loaded polyurethane polymer, rosin and graphite powder, performing melt spinning, adding the obtained polymeric fiber into an ethanol solution to prepare porous polymeric fiber, adding the porous polymeric fiber into a flame-retardant glue solution, dipping to obtain flame-retardant polymeric fiber, and spinning and weaving the flame-retardant polymeric fiber to obtain the flame-retardant wear-resistant fabric. According to the invention, the flame-retardant wear-resistant performance of the polyurethane resin is improved by compounding magnesium hydroxide in the polyurethane resin, and then the polyurethane fiber is subjected to porous modification, so that the prepared flame-retardant glue solution can be coated on the surface of the fiber and filled in the pore channel of the fiber, the content of the flame-retardant glue solution in the fiber is improved, and the flame-retardant glue solution contains a large amount of boron and phosphorus elements, so that the flame-retardant glue solution can perform a synergistic effect with the magnesium hydroxide in the polyurethane fiber, and the flame-retardant performance of the fiber is improved.
Description
Technical Field
The invention belongs to the field of curtain preparation, and relates to a preparation method of a flame-retardant wear-resistant curtain.
Background
The fabric curtain is usually made of cotton gauze, polyester fabric, polyester-cotton blended fabric, cotton-hemp blended fabric or non-woven fabric, and is used for shading sun, insulating heat and adjusting light, because the indoor coverage area of the curtain is large, when a fire disaster happens, large-area combustion is particularly easy to cause, the flame retardant property of the fabric curtain is emphasized, and meanwhile, because the curtain is frequently opened and closed, the curtain is frequently rubbed with a wall, and the curtain is easily abraded.
In the existing preparation process of the flame-retardant wear-resistant cloth, the cloth or yarn is usually directly immersed in the phosphorus flame retardant, or the fiber is directly doped with the inorganic flame retardant, so that the flame retardant is less dispersed in the cloth and has lower flame-retardant property.
Disclosure of Invention
The invention aims to provide a preparation method of a flame-retardant wear-resistant curtain, which is characterized in that magnesium hydroxide is compounded in polyurethane resin to improve the flame-retardant wear-resistant performance of the flame-retardant wear-resistant curtain, and then polyurethane fiber is subjected to porous modification, so that the prepared flame-retardant glue solution can be coated on the surface of fiber and filled in pore channels of the fiber, the content of the flame-retardant glue solution in the fiber is improved, and the flame-retardant glue solution contains a large amount of boron and phosphorus elements and can perform synergistic action with the magnesium hydroxide in the polyurethane fiber to improve the flame-retardant performance of the fiber, thereby solving the problems that cloth or yarn is usually directly soaked in a phosphorus flame retardant in the preparation process of the conventional flame-retardant wear-resistant cloth, or inorganic flame retardant is directly doped in the fiber, so that the flame retardant is less dispersed in the cloth and has lower flame-retardant performance; meanwhile, although the flame-retardant fiber is subjected to porous modification, the porous fiber is soaked in the flame-retardant glue solution, the flame-retardant glue solution is filled in fiber gaps, and the flame-retardant glue solution is of a hyperbranched polymer structure and has certain viscosity and toughness, so that the strength of the fiber reduced due to porous modification can be filled, and the wear resistance and mechanical property of the prepared flame-retardant fiber are not reduced while the flame-retardant property is improved.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a flame-retardant wear-resistant curtain comprises the following specific preparation processes:
firstly, heating low-melting-point polyurethane resin to 80 ℃, stirring and dissolving, then adding a sodium bicarbonate solution, adjusting the pH to 11, then dropwise adding a 30-35% magnesium nitrate solution into a reaction container while stirring, stopping dropwise adding when white precipitates are generated, then stirring and reacting at constant temperature for 10-20min, then heating to 100-105 ℃, stirring and reacting for 30-40min, washing and drying generated solid substances to obtain a loaded polyurethane polymer; the polyurethane resin is low-melting-point polyurethane resin with a melting point of 80 ℃, magnesium hydroxide is easily generated by magnesium ions precipitated in a solution with a pH value of 10, a large number of hydroxide ions exist in the magnesium hydroxide, and the hydroxide ions can be combined with amino groups in the polyurethane through hydrogen bond action at high temperature, so that the magnesium hydroxide is loaded on the polyurethane, and the unloaded magnesium hydroxide is directly washed away, so that the polyurethane has certain flame retardant property;
and step two, mixing the load polyurethane polymer prepared in the step one and rosin according to a mass ratio of 1: 0.43-0.45, adding into an open mill at the temperature of 135-; wherein 0.085-0.089g of graphite powder is added into each gram of the loaded polyurethane polymer;
thirdly, adding the polymeric fiber prepared in the second step into an ethanol solution, oscillating for 5-6h in an ultrasonic oscillation box at 50-55 ℃, fishing out, washing for 3-5 times by using ethanol, and drying in a drying chamber at 50-60 ℃ to obtain the porous polymeric fiber; the polymerized fiber yarn mainly contains polyurethane and rosin which are mixed, the rosin is easy to dissolve in an ethanol solution, the rosin in the polymerized fiber yarn is dissolved in the ethanol by adding the ethanol, the position of the rosin in the polymerized fiber yarn is originally vacated, so that a porous structure appears on the fiber yarn, and meanwhile, the polyurethane has certain bonding property, so that graphite powder can be bonded with the polyurethane and fixed, the graphite powder is uniformly fixed on the polymerized fiber yarn, and the conductivity and the wear resistance of the polymerized fiber yarn are improved;
fourthly, adding the porous polymeric fiber prepared in the third step into a flame-retardant glue solution, soaking for 3-5min, taking out, drying to obtain flame-retardant polymeric fiber, spinning the flame-retardant polymeric fiber into yarn, and spinning the yarn to obtain flame-retardant wear-resistant cloth for preparing the flame-retardant wear-resistant curtain; because the porous polymeric fiber contains a large number of pore channels, after the flame-retardant colloid is added, the colloid covers the surface of the fiber, and part of the colloid is filled in the pore channels of the fiber, so that the flame retardance of the interior and the surface of the fiber is realized, and the flame retardant property of the fiber is improved;
the flame-retardant glue solution is prepared by the following specific steps:
step 1: adding p-methoxybenzyl alcohol into diethyl ether, uniformly mixing, heating to 50-60 ℃, then dropwise adding a phosphoric acid solution, completely adding the phosphoric acid solution, heating to 85-90 ℃, carrying out reflux reaction for 5-6 hours, then washing a product with saturated sodium chloride, adding the product into ethyl acetate for extraction, and carrying out reduced pressure distillation on the obtained oil phase to obtain a product A; wherein the molar ratio of p-methoxybenzyl alcohol to phosphoric acid is 3: mixing at a ratio of 0.96-0.97; each phosphoric acid molecule can be grafted with three p-methoxybenzyl alcohols in three directions, so that branched phosphate taking phosphoric acid as a center is formed, and the phosphoric acid has a certain flame retardant property;
step 2: adding the product A prepared in the step 1 into a 33-35% hydrogen bromide acetic acid solution, heating to 100-35 ℃, performing reflux reaction at 120 ℃ for 10-12h to obtain a viscous product, washing the product with saturated sodium chloride, adding the product into acetone for extraction, and performing reduced pressure distillation on the obtained oil phase to obtain a product B; the product A is subjected to reflux reaction in a hydrogen bromide solution, wherein ether bonds are broken to generate phenolic hydroxyl groups, so that an action site is provided for later-stage reaction;
and step 3: adding the product B prepared in the step 2 into acetone, heating to 50-60 ℃, simultaneously adding 5% boric acid solution into the acetone while stirring, stirring at constant temperature for reacting for 3-4h after complete dripping to obtain a viscous product, and then heating to 100-105 ℃ to remove the solvent in the viscous product to obtain the flame-retardant polymer; wherein 0.12-0.15mL of 5% boric acid solution is added into each gram of the product B; the phenolic hydroxyl in the product B can be polymerized with boric acid, and the product B is a branched structure and is polymerized with three hydroxyl in the boric acid in three directions to form a hyperbranched polymer, so that the dissolving and dispersing performance of the polymer is improved, and meanwhile, the prepared polymer is prepared by polymerizing a large number of monomers taking a phosphorus element as a center from a large number of boron elements as the center to the periphery, so that the prepared polymer contains a large number of boron elements and phosphorus elements, when the polymer is coated on the surface of a fiber filament and filled in a pore channel of the fiber filament, the boron elements in the polymer generate boron oxide at high temperature, part of oxygen on the surface of the fiber filament is consumed, meanwhile, oxygen and heat are prevented from entering the fiber filament, the flame retardant performance is realized, meanwhile, phosphate contained in the polymer is decomposed into free radicals in a gas phase, and H & lt & gtand & gtOH free radicals generated by material combustion can be captured, the combustion reaction is interrupted, and the moisture generated in the combustion process can reduce the temperature of the system, further realize the flame-retardant effect, meanwhile, the magnesium hydroxide loaded in the fiber filament is decomposed at high temperature to release crystal water and absorb a large amount of heat, the temperature rise of the fiber filament is inhibited, the flame retardant property is further realized, the high-efficiency flame-retardant performance of the fiber yarn is realized through the synergistic effect of boron and phosphorus on the surface and in the inner pore canal of the fiber yarn, meanwhile, the problem of the whole fiber yarn matrix is reduced through the heat absorption effect of the magnesium hydroxide in the fiber yarn polymer, the flame retardant property is further realized, and because the water generated after the magnesium hydroxide inside the polymer is decomposed by heating is sealed inside the polymer, when the temperature is reduced, the generated water continuously reacts with the magnesium oxide to generate magnesium hydroxide, so that continuous and effective flame retardance can be realized, and the continuity of flame retardance can be improved;
and 4, step 4: adding the flame-retardant polymer prepared in the step 3 into an acetone solution, heating to 50-55 ℃, stirring and dissolving to obtain a viscous flame-retardant glue solution; wherein 2.85-2.91mL of acetone is added per gram of flame retardant polymer.
The invention has the beneficial effects that:
according to the invention, the flame-retardant wear-resistant performance of the flame-retardant wear-resistant fabric is improved by compounding magnesium hydroxide in polyurethane resin, and then the polyurethane fiber is subjected to porous modification, so that the prepared flame-retardant glue solution can be coated on the surface of the fiber and filled in the pore channel of the fiber, the content of the flame-retardant glue solution in the fiber is improved, and the flame-retardant glue solution contains a large amount of boron and phosphorus elements, so that the flame-retardant performance of the fiber can be improved by the synergistic effect of the flame-retardant glue solution and the magnesium hydroxide in the polyurethane fiber, and the problems that in the preparation process of the conventional flame-retardant wear-resistant fabric, the fabric or yarn is usually directly soaked in a phosphorus flame retardant, or an inorganic flame retardant is directly doped in the fiber, so that the flame retardant is less dispersed in the fabric, and the flame retardant performance is lower are solved.
Although the flame-retardant fiber is subjected to porous modification, the porous fiber is soaked in the flame-retardant glue solution, the flame-retardant glue solution is filled in fiber gaps, the flame-retardant glue solution is of a hyperbranched polymer structure and has certain viscosity and toughness, and the strength of the fiber reduced due to porous modification can be filled, so that the wear resistance and mechanical property of the prepared flame-retardant fiber are not reduced while the flame resistance is improved, and the problem that the mechanical property and wear resistance of the fiber modified through the through holes are reduced is effectively solved.
The polyurethane fiber matrix used in the invention has high toughness and wear resistance, magnesium ions are added into a polyurethane resin melt, wherein the magnesium ions are easy to precipitate in a solution with the pH value of 10 to generate magnesium hydroxide, a large number of hydroxide ions exist in the magnesium hydroxide, and the hydroxide ions can be combined with amino groups in the polyurethane at high temperature through hydrogen bond action, so that the magnesium hydroxide is loaded on the polyurethane, and the unloaded magnesium hydroxide is directly washed away, so that the polyurethane has a certain lasting flame retardant property, and meanwhile, the addition of the magnesium hydroxide inorganic filler and graphite powder can further improve the breaking strength and wear resistance of the fiber.
The flame-retardant colloid prepared by the invention is prepared by polymerizing a large amount of monomers taking phosphorus as the center to the periphery by taking a large amount of boron as the center, so that the prepared polymer contains a large amount of boron and phosphorus, when the polymer is coated on the surface of the fiber and filled in the pore channel of the fiber, the boron in the flame-retardant colloid generates boron oxide at high temperature, partial oxygen on the surface of the fiber is consumed, oxygen and heat are prevented from entering the fiber, the flame-retardant performance is realized, meanwhile, the contained phosphate is decomposed into free radicals in gas phase, H & ltOH & gt and OH & lt free radicals generated by material combustion can be captured, the combustion reaction is interrupted, the moisture generated in the combustion process can reduce the system temperature, the flame-retardant effect is further realized, meanwhile, the magnesium hydroxide loaded in the fiber decomposes at high temperature to release crystal water and absorb a large amount of heat, the temperature rise of the fiber is inhibited, the flame retardant performance is further realized, the high-efficiency flame retardant performance of the fiber is realized through the synergistic effect of boron and phosphorus on the surface of the fiber and in an internal pore passage, meanwhile, the problem of the whole fiber matrix is reduced through the heat absorption effect of magnesium hydroxide in the fiber polymer, the flame retardant performance is further realized, and because the water generated after the magnesium hydroxide in the polymer is heated and decomposed is sealed in the polymer, the water generated when the temperature is reduced continuously reacts with magnesium oxide to generate magnesium hydroxide, the continuous effective flame retardant can be realized, and the continuity of the flame retardant performance is improved.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a reaction formula of product A of the present invention;
FIG. 2 is a reaction formula of product B of the present invention;
FIG. 3 is a reaction structure of the flame retardant polymer.
Detailed Description
Referring to FIGS. 1-3, the following embodiments are illustrated in detail:
example 1:
the flame-retardant glue solution is prepared by the following specific steps:
step 1: adding 414g of p-methoxybenzyl alcohol into 2L of diethyl ether, uniformly mixing, heating to 50-60 ℃, then dropwise adding 94.08g of phosphoric acid, heating to 85-90 ℃ after complete addition, carrying out reflux reaction for 5-6h, then washing a product with saturated sodium chloride, adding the product into ethyl acetate for extraction, and carrying out reduced pressure distillation on the obtained oil phase to obtain a product A; wherein the molar ratio of p-methoxybenzyl alcohol to phosphorus pentoxide is 3: mixing at a ratio of 0.48-0.49;
step 2: adding 1kg of the product A prepared in the step 1 into 25mL of 33-35% hydrogen bromide acetic acid solution, heating to 100-120 ℃ for reflux reaction for 10-12h to obtain a viscous product, washing the product with saturated sodium chloride, adding the product into acetone for extraction, and then carrying out reduced pressure distillation on the obtained oil phase to obtain a product B;
and step 3: adding 1kg of the product B prepared in the step 2 into 20L of acetone, heating to 50-60 ℃, simultaneously adding 120mL of 5% boric acid solution into the acetone while stirring, stirring at constant temperature after complete dripping to obtain a viscous product, heating to 100-105 ℃, and removing the solvent to obtain the flame-retardant polymer; wherein 0.12-0.15mL of 5% boric acid solution is added into each gram of the product B;
and 4, step 4: and (3) adding 1kg of the flame-retardant polymer prepared in the step (3) into 2.85L of acetone solution, heating to 50-55 ℃, and stirring to dissolve to obtain viscous flame-retardant glue solution.
Example 2:
the specific preparation process of the flame retardant glue solution is as follows:
step 1: adding 276g of p-methoxybenzyl alcohol into 2L of diethyl ether, uniformly mixing, heating to 50-60 ℃, then adding 94.08g of phosphoric acid dropwise, heating to 85-90 ℃ after complete addition, carrying out reflux reaction for 5-6h, then washing a product with saturated sodium chloride, adding the product into ethyl acetate for extraction, and carrying out reduced pressure distillation on the obtained oil phase to obtain a product A;
step 2: adding 1kg of the product A prepared in the step 1 into 25mL of 33-35% hydrogen bromide acetic acid solution, heating to 100-120 ℃ for reflux reaction for 10-12h to obtain a viscous product, washing the product with saturated sodium chloride, adding the product into acetone for extraction, and then carrying out reduced pressure distillation on the obtained oil phase to obtain a product B;
and step 3: 1kg of the product B prepared in step 2 was added to 20L of acetone, the temperature was raised to 50 to 60 ℃ and 120mL of 5% boric acid solution was added thereto while stirring dropwise, to give a solid product which was insoluble in solvents such as acetone and dimethyl sulfoxide.
Example 3:
the specific preparation process of the flame retardant glue solution is as follows:
step 1: adding 414g of p-methoxybenzyl alcohol into 2L of diethyl ether, uniformly mixing, heating to 50-60 ℃, then dropwise adding 94.08g of phosphoric acid, heating to 85-90 ℃ after complete addition, carrying out reflux reaction for 5-6h, then washing a product with saturated sodium chloride, adding the product into ethyl acetate for extraction, and carrying out reduced pressure distillation on the obtained oil phase to obtain a product A;
step 2: adding 1kg of the product A prepared in the step 1 into 25mL of 33-35% hydrogen bromide acetic acid solution, heating to 100-120 ℃ for reflux reaction for 10-12h to obtain a viscous product, washing the product with saturated sodium chloride, adding the product into acetone for extraction, and then carrying out reduced pressure distillation on the obtained oil phase to obtain a product B;
and step 3: adding 1kg of the product B prepared in the step 2 into 20L of acetone, heating to 50-60 ℃, simultaneously adding 70mL of formaldehyde solution, stirring while dropwise adding, stirring at constant temperature for reacting for 3-4h after completely dropwise adding to obtain a viscous product, and then heating to 100-105 ℃ to remove the solvent therein to obtain the flame-retardant polymer;
and 4, step 4: adding 1kg of the flame-retardant polymer prepared in the step 3 into 2.9L of acetone solution, heating to 50-55 ℃, stirring and dissolving to obtain viscous glue solution.
Example 4:
a preparation method of a flame-retardant wear-resistant curtain comprises the following specific preparation processes:
firstly, heating low-melting-point polyurethane resin to 80 ℃, stirring and dissolving, then adding a sodium bicarbonate solution, adjusting the pH to 11, then dropwise adding a 30-35% magnesium nitrate solution into a reaction container while stirring, stopping dropwise adding when white precipitates are generated, then stirring and reacting at constant temperature for 10-20min, then heating to 100-105 ℃, stirring and reacting for 30-40min, washing and drying generated solid substances to obtain a loaded polyurethane polymer;
secondly, simultaneously adding 1kg of the loaded polyurethane polymer prepared in the first step and 0.43kg of rosin into an open mill at the temperature of 135-140 ℃ for refining for 10-15min, then adding 85g of graphite powder into the melt, and performing melt spinning on the melt after smelting for 3-5min to obtain polymeric fiber filaments;
thirdly, adding the polymeric fiber prepared in the second step into an ethanol solution, oscillating for 5-6h in an ultrasonic oscillation box at 50-55 ℃, fishing out, washing for 3-5 times by using ethanol, and drying in a drying chamber at 50-60 ℃ to obtain the porous polymeric fiber;
and fourthly, adding the porous polymeric fiber prepared in the third step into the flame-retardant glue solution prepared in the example 1, soaking for 3-5min, taking out, drying to obtain the flame-retardant polymeric fiber, spinning the flame-retardant polymeric fiber into yarns, and spinning the yarns to obtain the flame-retardant wear-resistant fabric for preparing the flame-retardant wear-resistant curtain.
Example 5:
a method for preparing a flame-retardant wear-resistant curtain, which has the same specific preparation process as that of example 4, wherein the flame-retardant glue solution prepared in example 1 and used in the fourth step in example 4 is replaced by the flame-retardant glue solution prepared in example 3.
Example 6:
a preparation method of a flame-retardant wear-resistant curtain comprises the following specific preparation processes:
firstly, heating low-melting-point polyurethane resin to 80 ℃, stirring and dissolving, then adding a sodium bicarbonate solution, adjusting the pH to 11, then dropwise adding a 30-35% magnesium nitrate solution into a reaction container while stirring, stopping dropwise adding when white precipitates are generated, then stirring and reacting at constant temperature for 10-20min, then heating to 100-105 ℃, stirring and reacting for 30-40min, washing and drying generated solid substances to obtain a loaded polyurethane polymer;
secondly, adding 1kg of the loaded polyurethane polymer prepared in the first step and 85g of graphite powder into an open mill at the temperature of 135-140 ℃ for refining for 10-15min, and carrying out melt spinning on the melt to obtain polymeric fiber yarns;
and thirdly, adding the polymeric fiber yarn prepared in the second step into the flame-retardant glue solution prepared in the embodiment 1, soaking for 3-5min, taking out, drying to obtain the flame-retardant polymeric fiber yarn, spinning the flame-retardant polymeric fiber yarn into yarn, and spinning the yarn to obtain the flame-retardant wear-resistant fabric for preparing the flame-retardant wear-resistant curtain.
Example 7:
a preparation method of a flame-retardant wear-resistant curtain comprises the following specific preparation processes:
firstly, simultaneously adding 1kg of polyurethane resin and 0.43kg of rosin into an open mill at the temperature of 135-140 ℃ for refining for 10-15min, then adding 85g of graphite powder into a melt, and carrying out melt spinning on the melt after smelting for 3-5min to obtain polymeric fiber yarns;
secondly, adding the polymeric fiber prepared in the first step into an ethanol solution, oscillating for 5-6h in an ultrasonic oscillation box at 50-55 ℃, fishing out, washing for 3-5 times by using ethanol, and drying in a drying chamber at 50-60 ℃ to obtain porous polymeric fiber;
and thirdly, adding the porous polymeric fiber prepared in the second step into the flame-retardant glue solution prepared in the embodiment 1, soaking for 3-5min, taking out, drying to obtain the flame-retardant polymeric fiber, spinning the flame-retardant polymeric fiber into yarn, and spinning the yarn to obtain the flame-retardant wear-resistant fabric for preparing the flame-retardant wear-resistant curtain.
Example 8:
a preparation method of a flame-retardant wear-resistant curtain is the same as that in example 4, and 0.43kg of rosin added in the second step in example 4 is replaced by 0.52kg of rosin.
Example 9:
a preparation method of a flame-retardant wear-resistant curtain is the same as that in example 4, and 0.43kg of rosin added in the second step in example 4 is replaced by 0.35kg of rosin.
Example 10:
the method comprises the steps of (1) measuring the mechanical property of the flame-retardant polymer fiber prepared in the examples 4-9, fixing one end of a fiber by a Zwiggle G522 type abrasion resistance tester, bypassing a friction roller and a fixing roller, hanging a weight with a certain weight at the other end of the fiber, applying a certain test tension to the fiber, coating the wrapping surface of the friction roller with metallographic abrasive paper, rotating the friction roller at a rotating speed of 400r/min to rub the fiber with each other, recording the time from the beginning of the rotation of the roller to the fiber fracture, dividing the time by the rotating speed of the friction roller to obtain the number of rotation turns at the fiber fracture, determining the friction property of the fiber through the number of rotation turns, wherein the larger the number of rotation turns is the higher the friction property, and the specific measurement result is shown in Table 1;
TABLE 1 measurement of mechanical Properties of flame-retardant polymeric filaments prepared in examples 4-9
As can be seen from Table 1, the fibers prepared in examples 4 and 5 have breaking strength of 17.13CN/dtex and breaking revolution of 1796r, the polyurethane has higher breaking strength and wear resistance, the wear resistance is further improved after compounding magnesium hydroxide, the wear resistance and tensile strength are improved by adding graphite powder, the fibers in example 6 are not subjected to porous modification, the fiber void degree is reduced in example 9, but the breaking strength and the breaking revolution are not greatly increased, the fibers in examples 4 and 5 are immersed in the flame-retardant glue solution in the preparation process, the flame-retardant glue solution is filled in fiber voids, the flame-retardant glue solution is of a hyperbranched polymer structure and has certain viscosity and toughness, the fibers can be filled with strength reduced by porous modification, but when the voids are increased too much in example 8, the flame retardant is viscous liquid, is easy to flow and cannot be completely filled in the flame retardant, so that the finally prepared fiber still has certain gaps, and the tensile strength and the abrasive breaking revolution number of the finally prepared fiber are reduced; in example 7, the abrasion resistance and breaking strength of the fiber were reduced because magnesium hydroxide was not added.
Example 11:
the flame-retardant fibers prepared in examples 4-9 were subjected to a limiting oxygen index test with reference to GB/T2406 + 1993 by using a high temperature oxygen index tester, and the specific measurement results are shown in Table 2:
table 2 oxygen limiting index test results for flame retardant fibers prepared in examples 4-9
As is apparent from Table 2, the limited oxygen index of the fiber prepared in example 4 reached 38.6, since the fiber prepared contained a large number of voids on the surface, the flame retardant colloid covered the surface of the fiber and filled the pores of the fiber, boron oxide was generated at high temperature by boron element in the polymer, part of oxygen on the surface of the fiber was consumed, and oxygen and heat were prevented from entering the fiber, achieving flame retardant property, and phosphate contained therein decomposed into radicals in the gas phase, which could trap H and OH radicals generated by the combustion of the material, interrupt the combustion reaction, and moisture generated during the combustion could lower the system temperature, further achieving flame retardant effect, while magnesium hydroxide loaded inside the fiber was decomposed at high temperature to release crystal water and absorb a large amount of heat, suppressing the rise of the fiber temperature, further achieving flame retardant property, the high-efficiency flame retardant property of the fiber yarn is realized through the synergistic effect of boron and phosphorus on the surface and in the inner pore canal of the fiber yarn, meanwhile, the problem of the whole fiber yarn matrix is reduced through the heat absorption effect of magnesium hydroxide in the polymer of the fiber yarn, the flame retardant property is further realized, and as the water generated after the magnesium hydroxide in the polymer is heated and decomposed is sealed in the polymer, the water generated continuously reacts with magnesium oxide to generate magnesium hydroxide when the temperature is reduced, the continuous and effective flame retardant property can be realized, and the continuity of the flame retardant property is improved; in example 5, the flame retardant colloid used in example 7 does not contain boron element, so that the flame retardant property is reduced, and the flame retardant colloid used in example 7 does not contain magnesium hydroxide, so that the flame retardant property of the fiber is reduced, therefore, it can be known that the high-efficiency flame retardant effect can be realized through the synergistic effect of the three, and in example 6, because the surface of the prepared fiber is not subjected to porous modification, the flame retardant colloid is directly coated on the surface of the fiber, and the fiber is not filled with the flame retardant colloid, so that the content of the flame retardant element in the fiber is greatly reduced, so that the flame retardant property of the fiber is reduced, and meanwhile, the surface of the flame retardant fiber prepared in example 8 has more pores, but the flame retardant is viscous liquid, is easy to flow and cannot be completely filled therein, so that the amount of the filled flame retardant colloid cannot be changed too much, so that the flame retardant property of the fiber is not increased too much, when the surface of the fiber is reduced in the gap of the example 9, the content of the filled flame-retardant glue solution is reduced, and the flame-retardant performance is greatly reduced.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. The preparation method of the flame-retardant wear-resistant curtain is characterized by comprising the following specific preparation processes:
heating low-melting-point polyurethane resin to 80 ℃, stirring and dissolving, then adding a sodium bicarbonate solution, adjusting the pH to 11, then dropwise adding a 30-35% magnesium nitrate solution into a reaction container while stirring, stopping dropwise adding when white precipitate is generated, then stirring and reacting at constant temperature for 10-20min, then heating to 100-105 ℃, stirring and reacting for 30-40min to obtain a solid substance, and washing and drying the generated solid substance to obtain a load polyurethane polymer;
secondly, simultaneously adding the loaded polyurethane polymer and rosin prepared in the first step into an open mill at the temperature of 135-140 ℃ for refining for 10-15min, then adding graphite powder into the melt, and performing melt spinning on the melt after smelting for 3-5min to obtain polymeric fiber yarns;
thirdly, adding the polymeric fiber prepared in the second step into an ethanol solution, oscillating for 5-6h in an ultrasonic oscillation box at 50-55 ℃, fishing out, washing for 3-5 times by using ethanol, and drying in a drying chamber at 50-60 ℃ to obtain the porous polymeric fiber;
fourthly, adding the porous polymeric fiber prepared in the third step into a flame-retardant glue solution, soaking for 3-5min, taking out, drying to obtain flame-retardant polymeric fiber, spinning the flame-retardant polymeric fiber into yarn, and spinning the yarn to obtain flame-retardant wear-resistant cloth for preparing the flame-retardant wear-resistant curtain;
the specific preparation process of the flame-retardant glue solution is as follows:
step 1: adding p-methoxybenzyl alcohol into diethyl ether, uniformly mixing, heating to 50-60 ℃, then dropwise adding a phosphoric acid solution, completely adding the phosphoric acid solution, heating to 85-90 ℃, carrying out reflux reaction for 5-6 hours, then washing a product with saturated sodium chloride, adding the product into ethyl acetate for extraction, and carrying out reduced pressure distillation on the obtained oil phase to obtain a product A;
step 2: adding the product A prepared in the step 1 into a 33-35% hydrogen bromide acetic acid solution, heating to 100-35 ℃, performing reflux reaction at 120 ℃ for 10-12h to obtain a viscous product, washing the product with saturated sodium chloride, adding the product into acetone for extraction, and performing reduced pressure distillation on the obtained oil phase to obtain a product B;
and step 3: adding the product B prepared in the step 2 into acetone, heating to 50-60 ℃, simultaneously adding 5% boric acid solution into the acetone while stirring, stirring at constant temperature for reacting for 3-4h after complete dripping to obtain a viscous product, and then heating to 100-105 ℃ to remove the solvent in the viscous product to obtain the flame-retardant polymer;
and 4, step 4: and (3) adding the flame-retardant polymer prepared in the step (3) into an acetone solution, heating to 50-55 ℃, stirring and dissolving to obtain a viscous flame-retardant glue solution.
2. The method for preparing a flame-retardant and wear-resistant curtain as claimed in claim 1, wherein 0.085-0.089g of graphite powder is added to each gram of the loaded polyurethane polymer in the second step.
3. The preparation method of the flame-retardant and wear-resistant curtain as claimed in claim 1, wherein the mass ratio of the polyurethane polymer and the rosin in the second step is 1: 0.43-0.45.
4. The preparation method of the flame-retardant wear-resistant curtain as claimed in claim 1, wherein in the step 1, the p-methoxybenzyl alcohol and the phosphoric acid are mixed according to a molar ratio of 3: mixing at a ratio of 0.96-0.97.
5. The method for preparing a flame-retardant and wear-resistant curtain as claimed in claim 1, wherein 0.12-0.15mL of 5% boric acid solution is added to each gram of product B in step 3.
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| CN110644238B (en) * | 2019-09-18 | 2022-04-19 | 界首市双鑫纺织有限公司 | Preparation process of wear-resistant fireproof cloth |
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