阅读说明：本技术 一种耐磨防火布料的制备工艺 (Preparation process of wear-resistant fireproof cloth ) 是由 杨双建 龚琤琤 于 2019-09-18 设计创作，主要内容包括：本发明公开了一种耐磨防火布料的制备工艺,具体制备过程如下：第一步,将变色聚合物加入丙酮溶液中搅拌溶解,然后向其中加入多孔聚苯酰胺磷酸酯纤维,常温下浸渍30-40min,然后进行过滤烘干；第二步,烘干后的多孔聚苯酰胺磷酸酯纤维在阻燃胶体中搅拌混合20-30min,然后进行烘干,并将烘干后的耐磨纤维纺织成纱线,然后将得到的纱线编制成布料,得到耐磨防火布料。本发明制备的多孔聚苯酰胺磷酸酯纤维本身具有一定的防火性,并且在纤维的表面和内部空隙中填充阻燃胶体,使得纤维的防火性能升高,实现了限位由内到外高强度防火作用。(The invention discloses a preparation process of wear-resistant fireproof cloth, which comprises the following specific preparation processes: firstly, adding a color-changing polymer into an acetone solution, stirring and dissolving, then adding porous polyphenyl amide phosphate ester fiber into the acetone solution, soaking for 30-40min at normal temperature, and then filtering and drying; and secondly, stirring and mixing the dried porous polybenzamide phosphate fibers in a flame-retardant colloid for 20-30min, then drying, spinning the dried wear-resistant fibers into yarns, and weaving the obtained yarns into cloth to obtain the wear-resistant fireproof cloth. The porous polyphenyl amide phosphate fiber prepared by the invention has certain fire resistance, and the surface and the inner gaps of the fiber are filled with the flame-retardant colloid, so that the fire resistance of the fiber is improved, and the high-strength fire prevention effect of limiting from inside to outside is realized.)

1. A preparation process of wear-resistant fireproof cloth is characterized by comprising the following specific preparation processes:

firstly, adding a color-changing polymer into an acetone solution, stirring and dissolving, then adding porous polyphenyl amide phosphate ester fiber into the acetone solution, soaking for 30-40min at normal temperature, and then filtering and drying;

and secondly, stirring and mixing the dried porous polybenzamide phosphate fibers in a flame-retardant colloid for 20-30min, then drying, spinning the dried wear-resistant fibers into yarns, and weaving the obtained yarns into cloth to obtain the wear-resistant fireproof cloth.

2. The preparation process of the wear-resistant fireproof cloth material according to claim 1, wherein the porous polybenzamide phosphate fiber is prepared by the following specific steps: weighing a certain amount of glycerol, adding the glycerol into ether, stirring and mixing to form a transparent dilute solution, then dropwise adding polyisocyanate adhesive into a reaction vessel at normal temperature, and stirring and reacting for 4-5 hours after the polyisocyanate adhesive is completely dropwise added to obtain a polymer solution; adding 90-95mL of diethyl ether into each mole of glycerol; heating the polymer solution to 65-70 ℃, adding paraffin into the polymer solution, stirring and dissolving the paraffin in the polymer solution to obtain spinning solution; spinning the spinning solution by an electrostatic spinning machine to obtain the poly (phenyl amide phosphate) composite fiber yarn; and fourthly, adding the polyphenyl amide composite fiber into 80 ℃ hot water, cooking for 5-10min, fishing out, drying, adding the dried fiber into 80 ℃ hot water again, cooking for 5-10min, fishing out, repeatedly cooking for 6-7 times, and drying to obtain the porous polyphenyl amide phosphate fiber.

3. The preparation process of the wear-resistant fireproof cloth according to claim 2, wherein the polymer solution and the paraffin in the step (II) are mixed according to a mass ratio of 1: mixing at a ratio of 0.1.

4. The preparation process of the wear-resistant fireproof cloth material according to claim 1, wherein the specific preparation process of the color-changing polymer is as follows:

step 1: adding urea into water, stirring and dissolving, adding salicylaldehyde, stirring and reacting for 2-3h at normal temperature, and then carrying out reduced pressure distillation to obtain a product A;

step 2: acetic acid and concentrated sulfuric acid are mixed according to the volume ratio of 5: 1 to form an acid solvent, adding the acid solvent into a reaction container, cooling to 8-10 ℃, adding 37 mass percent of formaldehyde and n-hexylamine, stirring at a constant temperature for 10-15min, adding the product A prepared in the step 1 into the reaction container, keeping the temperature constant, reacting for 2-3h, heating to 30-35 ℃, stirring and reacting for 8-9h to obtain a polymer solution, adding the obtained polymer solution into ice water, stirring and mixing for 30-40min to precipitate solids, filtering, washing a filter cake to be neutral, adjusting the filtrate to be neutral by using ammonia water, standing to precipitate solids, filtering the precipitated solids, and drying the filtered solids together with the washed filter cake to obtain the color-changing polymer.

5. The preparation process of the wear-resistant fireproof cloth according to claim 4, wherein in the step 2, 5.4-5.7g of formaldehyde solution, 7-8mL of acid solvent and 0.63-0.64g of n-hexylamine are added to each gram of the product A.

6. The process of claim 1, wherein in the second step, 12-13mL of acetone solution is added to each gram of the color-changing polymer, and 1g of porous polybenzamide phosphate fiber is added.

7. The preparation process of the wear-resistant fireproof fabric according to claim 1, wherein the flame retardant colloid is prepared by the following steps: adding the liquid phenolic resin into a stirring kettle, simultaneously adding the polyisocyanate adhesive into the stirring kettle, and stirring and reacting for 1-2h at normal temperature to obtain viscous colloidal solution.

8. The preparation process of the wear-resistant fireproof cloth according to claim 7, wherein 1.23-1.25g of polyisocyanate adhesive is added to each gram of liquid phenolic aldehyde.

Technical Field

The invention belongs to the field of fabric preparation, and relates to a preparation process of a wear-resistant fireproof fabric.

Background

In the fire control work, the fire fighter works under high temperature, and the temperature that the human body can move under high temperature is limited, and work can cause life danger under high temperature for a long time, and current fire control dress has certain fire behavior at that time, but the temperature condition in the environment that can not effectual real-time detection locates for the fire fighter can not be according to the temperature variation vigilant in high temperature environment.

Disclosure of Invention

The invention aims to provide a preparation process of wear-resistant fireproof cloth, which comprises the steps of preparing porous polyphenyl amide phosphate fiber, impregnating color-changing polymer on the surface and inside of the fiber, filling and sealing the fiber by flame-retardant colloid, wherein the color-changing performance of the fiber cannot be weakened due to long-term washing due to the flame-retardant colloid; meanwhile, the color-changing temperature of the color-changing polymer is low, after the flame-retardant colloid is coated on the surface of the color-changing polymer, the color-changing temperature is increased to 56 ℃ through the isolation of the colloid, so that the fabric can change color at high temperature, and the high temperature can be warned to prevent the damage to the human body.

The purpose of the invention can be realized by the following technical scheme:

a preparation process of wear-resistant fireproof cloth comprises the following specific preparation processes:

in the first step, the specific preparation process of the porous polybenzamide phosphate fiber is as follows: weighing a certain amount of glycerol, adding the glycerol into ether, stirring and mixing to form a transparent dilute solution, then dropwise adding polyisocyanate adhesive into a reaction vessel at normal temperature, and stirring and reacting for 4-5 hours after the polyisocyanate adhesive is completely dropwise added to obtain a polymer solution; wherein the ratio of the glycerol to the polyisocyanate glue is 3: 1, adding 90-95mL of diethyl ether into each mole of glycerol; because the polyisocyanate adhesive is characterized in that a phosphate group is taken as a center, three phenylisocyanate groups are crosslinked at the side, the isocyanate groups can react with alcoholic hydroxyl groups in glycerol to be crosslinked, the glycerol contains three hydroxyl groups, and meanwhile, the polyisocyanate adhesive contains three isocyanate groups in three different directions, so that the prepared polymer has a branched structure, is difficult to agglomerate and can be uniformly dispersed, and meanwhile, an amide group generated after polymerization has certain water absorption, so that the water absorption performance of the prepared polymer is improved; because the polyisocyanate adhesive takes phosphate groups as the center, the polymer generated after polymerization contains a large amount of phosphate groups, thereby improving the fire resistance of the polymer; heating the polymer solution to 65-70 ℃, adding paraffin into the polymer solution, stirring and dissolving the paraffin in the polymer solution to obtain spinning solution; the polymer solution and the paraffin are mixed according to the mass ratio of 1: mixing at a ratio of 0.1; spinning the spinning solution by an electrostatic spinning machine to obtain the poly (phenyl amide phosphate) composite fiber yarn; adding the polyphenyl amide composite fiber into 80 ℃ hot water, cooking for 5-10min, fishing out, drying, adding the dried fiber into 80 ℃ hot water again, cooking for 5-10min, fishing out, repeatedly cooking for 6-7 times, and drying to obtain porous polyphenyl amide phosphate fiber, and simultaneously fully melting paraffin in the fiber in water, wherein a large amount of gaps are formed on the surface and inside of the obtained fiber;

in the second step, the preparation process of the color-changing polymer is as follows:

step 1: adding urea into water, stirring and dissolving, adding salicylaldehyde, stirring and reacting for 2-3h at normal temperature, and then carrying out reduced pressure distillation to obtain a product A; the urea contains two amino groups, so that the urea can be polymerized with aldehyde groups in the salicylaldehyde, so that the two salicylaldehyde are compounded on two sides of the urea, and the amino groups and the aldehyde groups react to generate-C-N-; wherein the ratio of urea to salicylaldehyde is 1: 2, mixing and preparing;

step 2: acetic acid and concentrated sulfuric acid are mixed according to the volume ratio of 5: 1 to form an acid solvent, adding the acid solvent into a reaction container, cooling to 8-10 ℃, adding 37 mass percent of formaldehyde and n-hexylamine, stirring at a constant temperature for 10-15min, adding the product A prepared in the step 1 into the reaction container, keeping the temperature constant, reacting for 2-3h, heating to 30-35 ℃, stirring and reacting for 8-9h to obtain a polymer solution, adding the obtained polymer solution into ice water, stirring and mixing for 30-40min to precipitate solids, filtering, washing a filter cake to be neutral, adjusting the filtrate to be neutral by using ammonia water, standing to precipitate solids, filtering the precipitated solids, and drying the filtered solids together with the washed filter cake to obtain a color-changing polymer; adding 5.4-5.7g of formaldehyde solution into each gram of the product A, adding 7-8mL of acid solvent, adding 0.63-0.64g of N-hexylamine, wherein hydroxyl in the aromatic compound has stronger ortho-para activity, and the meta-position activity of-C ═ N-is stronger, so that the phenolic hydroxyl para-position in the product A, namely the meta-position of-C ═ N-, has higher activity under the action of the two, and can generate Mannich reaction with formaldehyde and amine; because-C ═ N-in the generated product is in an ortho position with phenolic hydroxyl and has intramolecular hydrogen bonds, when the temperature is increased, proton hydrogen in the phenolic hydroxyl is transferred to nitrogen atoms, so that intramolecular rapid and reversible hydrogen transfer reaction is caused, the enol form of the polymer is changed into a ketone structure, the color is also reversibly changed, and simultaneously, because a large amount of-C ═ N-is contained in the polymer, a large amount of enol form can be generated, the color change temperature of the prepared color change polymer solution is low, the color change can be realized at 42 ℃, and the polymer is changed from earthy yellow to bright red;

thirdly, adding the color-changing polymer into an acetone solution, stirring and dissolving, then adding the porous polyphenyl amide phosphate fiber into the acetone solution, soaking for 30-40min at normal temperature, and then filtering and drying; wherein, 12-13mL of acetone solution is added into each gram of the color-changing polymer, and 1g of porous polybenzamide phosphate fiber is added; because the porous polybenzamide phosphate fiber has higher water absorption, a large amount of color-changing polymer solution is soaked in the porous polybenzamide phosphate fiber after the color-changing polymer solution is soaked in the color-changing polymer solution;

fourthly, adding the liquid phenolic resin into a stirring kettle, simultaneously adding the polyisocyanate adhesive into the stirring kettle, and stirring and reacting for 1-2 hours at normal temperature to obtain viscous colloidal solution; wherein 1.23-1.25g of polyisocyanate adhesive is added into each gram of liquid phenolic aldehyde; the phenolic resin contains phenolic hydroxyl, and can be polymerized with isocyanate groups in polyisocyanate glue, three isocyanate groups in the polyisocyanate glue are positioned in three different directions, so that the phenolic resin forms a branched structure in a crosslinking process, the crosslinking degree of the phenolic resin is further reduced, and a polymer generated after crosslinking contains a large amount of phosphate groups, so that the colloid has a certain flame retardant property, and is prepared by crosslinking the phenolic resin, the prepared colloid has high cohesiveness, can be firmly adhered and filled in gaps in the porous polybenzamide phosphate fibers, and can adhere and fix the color-changing polymer impregnated on the surfaces of the porous polybenzamide phosphate fibers, so that the color-changing polymer is prevented from being separated after the fibers are washed for a long time, and the color-changing property of the fibers is further reduced; the fiber has low wear resistance, the phenolic resin has high wear resistance, the wear resistance is further increased after polymerization, and the fiber is covered in the surface and inner pore channels of the fiber after curing and drying, so that the wear resistance of the fiber from inside to outside is increased, the prepared fiber has high wear resistance and toughness, and the color change performance cannot be weakened due to long-term washing; meanwhile, due to the fact that the color-changing temperature of the color-changing polymer is low, after the flame-retardant colloid is coated on the surface of the color-changing polymer, the color-changing temperature is raised to 56 ℃ through isolation of the colloid, so that the fabric can change color at high temperature, and can warn high temperature to prevent damage to a human body;

and fifthly, stirring and mixing the dried porous polyphenyl amide phosphate fibers in a flame-retardant colloid for 20-30min, then drying, spinning the dried wear-resistant fibers into yarns, and weaving the obtained yarns into cloth to obtain the wear-resistant fireproof cloth.

The invention has the beneficial effects that:

1. according to the invention, the porous polybenzamide phosphate fiber is prepared, and the surface and the interior of the fiber are impregnated with the color-changing polymer and then are filled and sealed by the flame-retardant colloid, so that the color-changing performance of the fiber is not weakened due to long-term washing due to the flame-retardant colloid; meanwhile, the color-changing temperature of the color-changing polymer is low, after the flame-retardant colloid is coated on the surface of the color-changing polymer, the color-changing temperature is increased to 56 ℃ through the isolation of the colloid, so that the fabric can change color at high temperature, and the high temperature can be warned to prevent the damage to the human body.

2. The color-changing polymer prepared by the invention contains a large amount of-C-N-groups, and-C-N-is in an ortho position with phenolic hydroxyl and has intramolecular hydrogen bonds, when the temperature is increased, proton hydrogen in the phenolic hydroxyl is transferred to nitrogen atoms to cause rapid and reversible hydrogen migration reaction in molecules, so that the polymer is changed from enol form to ketone form, the color is also reversibly changed, simultaneously, because the polymer contains a large amount of-C-N-, a large amount of enol form can be generated, the color-changing temperature of the prepared color-changing polymer solution is lower, the color change can be realized at 42 ℃, the polymer is changed from khaki to bright red, when the fiber surface is coated with flame-retardant colloid, the color-changing temperature is increased to 56 ℃ through the barrier effect of the colloid, the detection of high-temperature limit activity temperature can be realized, meanwhile, the flame-retardant colloid is coated to prevent the content of the color-changing polymer from being reduced after being washed for many times, and the color-changing performance is reduced or even disappears, so that the prepared fiber can change color at a high temperature of 56 ℃ and can effectively prevent the color-changing performance from disappearing.

3. The porous polyphenyl amide phosphate fiber prepared by the invention has certain fire resistance, and the surface and the inner gaps of the fiber are filled with the flame-retardant colloid, so that the fire resistance of the fiber is improved, and the high-strength fire prevention effect of limiting from inside to outside is realized.

4. The prepared porous polybenzamide phosphate fiber has a porous structure, so that the strength and the wear resistance of the fiber are reduced, but the flame-retardant colloid is filled in the surface and the gaps of the fiber, the phenolic resin has higher wear resistance, the wear resistance is further increased after polymerization, and the fiber is covered in the surface and the inner pore channels after curing and drying, so that the wear resistance of the fiber from inside to outside is increased, the prepared fiber has higher wear resistance and toughness, and further the prepared porous fiber can not only realize the condition of carrying a large amount of color-changing polymer, but also can not reduce the strength and the toughness of the fiber, and can improve the strength and the wear resistance of the fiber through the filling effect.

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 mechanism of color change of the color-changing polymer of the present invention.

Detailed Description

Referring to fig. 1, the following embodiments are described in detail: