CN111764171A - Phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification and preparation method thereof - Google Patents
Phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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Abstract
The invention relates to the field of textiles, and discloses a phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification and a preparation method thereof. According to the invention, by utilizing the self-polymerization characteristic of dopamine and the broad-spectrum viscosity of polydopamine, the phosphorus flame-retardant polyester fabric and the weak alkaline aqueous solution of dopamine are stirred in the air for self-polymerization to enable the surface of fabric fibers to be polymerized with a polydopamine layer, and then, a catechol group on the surface of the polydopamine is utilized as a post-treatment modification site to react and combine with a boric acid group in a boron anti-dripping agent under the weak alkaline condition, so that the boron anti-dripping agent is firmly combined on the surface of the flame-retardant fabric, and the bonding force is stronger compared with that of a conventional post-finishing mode, and the synergistic effect of flame retardance and anti-dripping can be achieved.
Description
Technical Field
The invention relates to the field of textiles, in particular to a phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification and a preparation method thereof.
Background
Polyethylene terephthalate (PET) has a large share of synthetic fibers due to its advantages of high modulus, high strength, high elasticity, shape retention, heat resistance, etc., and in recent years, it has been widely used in the fields of packaging, construction, automobiles, electronic and electrical appliances, medical health, etc., in addition to as a fiber material.
In recent years, China has become the first major polyester producing country in the world. The vast majority of the polyesters in China are used for preparing fibers, and are mainly conventional polyester fibers, and the polyesters have the problems of excessive yield, insufficient operation and the like, so that the profit of enterprises is reduced. On the other hand, the conventional polyester has certain limitation in application in some important fields due to inherent problems of inflammability, melt dripping and the like, and particularly, after the requirements on the combustion performance of flame-retardant products and components in public places and the issuance of national standards for marking are issued, the conventional polyester has attracted more attention as the flame-retardant and anti-melt dripping performance of polyester fibers which are widely applied in public places such as aviation, railways, hotels and the like. Therefore, the development of new flame-retardant and anti-dripping polyester products is imperative.
The most effective flame-retardant polyester fabric in the existing market is CEPPA copolymer type flame-retardant polyester fabric, and in actual use, although the product has a high oxygen index, the flame-retardant principle of melt drip promotion leads to the fact that the flame-retardant polyester can generate a large amount of melt drip phenomena during combustion, so that people can be scalded, secondary burn can be caused, and serious loss of lives and properties of people can be caused. In fact, most phosphorus flame retardants realize flame retardance by taking away heat through molten drops, so that the problem of mutual contradiction between flame retardance and molten drop resistance exists, and the research on flame-retardant and molten drop-resistant polyester becomes a difficult problem.
Disclosure of Invention
In order to solve the technical problems, the invention provides phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification and a preparation method thereof.
The specific technical scheme of the invention is as follows: a phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification comprises a polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fibers as raw materials, and polydopamine and boron series anti-dripping agents attached to the surface of the polyester fabric through an after-finishing method.
Preferably, the boron-based anti-dropping agent is a compound having the following structure:
preferably, the polyester fabric has a fiber specification of 75-300D, 48-144f and a phosphorus content of 4500-7000 ppm.
A preparation method of phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification comprises the following steps:
1) adding an oil removing agent into hot water, and adding polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fiber as a raw material into the hot water to remove oil.
The surface of the polyester fiber is provided with an oil agent layer, the oil agent layer cannot be directly attached to the surface of the fiber due to the hydrophilic substance of dopamine, and the oil agent on the surface of the polyester fiber can be removed after oil removal treatment, so that subsequent attachment of dopamine is facilitated.
2) And drying the polyester fabric after oil removal, adding the polyester fabric into a Tris-HCl buffer solution, adding a dopamine monomer, stirring, and realizing self-polymerization coating of dopamine by using oxygen in the air as a catalyst to obtain the poly-dopamine surface modified polyester fabric.
3) Adding the boron system anti-dripping agent into a Tris-HCl buffer solution, and uniformly stirring to obtain an after-finishing solution containing the boron system anti-dripping agent; dipping the polyester fabric obtained in the step 2) in the after-finishing liquid and stirring to carry out surface grafting reaction; and finally, taking out the polyester fabric, washing and drying to obtain a finished product.
According to the invention, by utilizing the self-polymerization characteristic of dopamine and the broad-spectrum viscosity of polydopamine, the phosphorus flame-retardant polyester fabric and the weak alkaline aqueous solution of dopamine are stirred in the air for self-polymerization to enable the surface of fabric fibers to be polymerized with a polydopamine layer, and then, a catechol group on the surface of the polydopamine is utilized as a post-treatment modification site to react and combine with a boric acid group in a boron anti-dripping agent under the weak alkaline condition, so that the boron anti-dripping agent is firmly combined on the surface of the flame-retardant fabric, and the bonding force is stronger compared with that of a conventional post-finishing mode, and the synergistic effect of flame retardance and anti-dripping can be achieved.
Preferably, in the step 1), the oil is removed by washing with water at 75-85 ℃.
Preferably, in the step 2), the concentration of the dopamine monomer in the Tris-HCl buffer solution is 1-4 g/L; the mass volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L.
Preferably, in step 2), the stirring time is 24-72 h.
Preferably, in step 2) and step 3), the Tris-HCl buffer has a pH of 8.2 to 8.8.
Preferably, in the step 3), the concentration of the boron-based anti-dropping agent in the Tris-HCl buffer solution is 1-6 g/L; the mass volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L.
Preferably, in step 3), the stirring time is 2-4 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts phosphorus flame-retardant polyester fabric on the market as base cloth, common dopamine as a modifying monomer and easily prepared boron anti-dropping agent as a modifier, and the raw materials are easy to obtain and low in cost.
2. The invention adopts dopamine with simple polymerization conditions as a modified monomer, further modifies the dopamine by utilizing the reaction of boric acid groups and catechol groups under alkaline conditions, does not need external heating, has mild reaction conditions and saves energy.
3. According to the invention, the boron-based anti-dripping agent is bonded to the polydopamine on the surface of the fabric in a covalent bonding manner, and the polydopamine has very strong broad-spectrum viscosity and very strong bonding force, compared with a conventional after-finishing agent, the polydopamine is bonded in fiber gaps through Van der Waals force in a conventional after-finishing process, and the polydopamine has stronger bonding force and better water washing resistance, and can stay on the surface of the fabric for a longer time.
4. According to the invention, the boron series anti-dropping agent is used for modification on the basis of the phosphorus series flame retardant polyester fabric, and an acid source provided during combustion of the phosphorus series flame retardant can promote the boron series anti-dropping agent to be dehydrated to form a glassy boron oxide compound, so that the glassy boron oxide compound is coated on the surface of the fabric, charring is promoted, dropping of molten liquid is prevented, and the flame-retardant anti-dropping agent has high-efficiency flame-retardant anti-dropping capability. That is, the boron-based anti-dripping agent alone does not have a very high anti-dripping effect in the present invention, and it is necessary to combine with the phosphorus-based flame retardant at the same time to exert a good anti-dripping property (see, for details, comparative example 3).
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification comprises a polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fibers as raw materials, and polydopamine and boron series anti-dripping agents attached to the surface of the polyester fabric through an after-finishing method. The polyester fabric has a fiber specification of 75-300D, 48-144f and a phosphorus content of 4500-7000 ppm. The boron-based anti-dropping agent is a compound with the following structure:
a preparation method of phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification comprises the following steps:
1) adding an oil removing agent into hot water, and adding polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fiber as a raw material into the hot water to remove oil. Washing with water at 75-85 deg.C to remove oil.
2) And drying the polyester fabric after oil removal, and adding the polyester fabric into a Tris-HCl buffer solution with the pH value of 8.2-8.8, wherein the mass-volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L. Then adding dopamine monomer until the concentration of the dopamine monomer is 1-4g/L, stirring for 24-72h, and realizing self-polymerization coating of dopamine by using oxygen in the air as a catalyst to obtain the poly-dopamine surface modified polyester fabric.
3) Adding the boron series anti-dropping agent into a Tris-HCl buffer solution with the pH value of 8.2-8.8, and stirring for 2-4h to obtain an after-finishing liquid containing the boron series anti-dropping agent with the concentration of 1-6 g/L; dipping the polyester fabric obtained in the step 2) in the after-finishing liquid and stirring to carry out surface grafting reaction; the mass volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L. And finally, taking out the polyester fabric, washing and drying to obtain a finished product.
Specific examples and comparative examples
Example 1
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 2g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, adding 2g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index was found to reach 33.6%. The cloth sample is vertically combusted, no melting dripping exists, the average damage length is 85mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the melting dripping number in 30s combustion is 22 drops.
Example 2
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 2g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 3g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 31.5%, the cloth sample is vertically combusted without melt dripping, the average damage length is 75mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the number of melt dripping in 30s of combustion is 19.
Example 3
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 2g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 4g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 30.6%, the cloth sample is vertically combusted without melt dripping, the average damage length is 65mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the melt dripping number in the 30s combustion is 15 drops.
Example 4
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 4g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 3g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 29.4%, the cloth sample is vertically combusted without melt dripping, the average damage length is 60mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the number of melt dripping in 30s of combustion is 14.
Example 5
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 4g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 3g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, repeatedly washing the cloth sample for ten times by using deionized water, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 29.0%, the cloth sample is vertically combusted without melt dripping, the average damage length is 65mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the number of melt dripping in 30s of combustion is 16.
Example 6
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 4g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 4g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 28.7%, the cloth sample is vertically combusted without melt dripping, the average damage length is 55mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the melt dripping number in the 30s combustion is 12 drops.
Example 7
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 4g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 4g of 1, 3-oxaborole (I) into the buffer solution, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under the mechanical stirring of 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample for ten times by using deionized water, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 28.4%, the cloth sample is vertically combusted without melt dripping, the average damage length is 58mm, the B1 level is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the number of melt dripping in 30s of combustion is 14.
Example 8
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 4g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 4g of bis (1, 3-oxaborole) amyl ether (II) of 1-2g, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 28.0%, the cloth sample is vertically combusted without melt dripping, the average damage length is 50mm, the B1 level is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the melt dripping number in the 30s combustion is 12 drops.
Example 9
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 2g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 2g of bis (1, 3-oxaborole) amyl ether (II) in 1-2g, adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to reach 33.2%, the cloth sample is vertically combusted without melt dripping, the average damage length is 83mm, the level B1 is reached, the same cloth sample is further wound into a compact rod shape to be subjected to a continuous vertical combustion test for 30s, and the number of melt dripping in 30s of combustion is 20 drops.
Comparative example 1
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
And taking out the cloth sample, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index was found to reach 34.5%. The cloth sample is vertically combusted, no melting dripping exists, the average damage length is 105mm, the same cloth sample is further wound into a compact rod shape to be subjected to a 30-second continuous vertical combustion test, and the number of the melting dripping in 30-second combustion is 28 drops.
Comparative example 2 (applying boron series anti-dropping agent by after-finishing)
Polyester fabric prepared from phosphorus-containing flame-retardant polyester fiber (fiber specification of 150D/72f, phosphorus content of 6500ppm, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Preparing 1, 3-oxaborole (I) into 3% emulsion by using deionized water, padding two deoiled cloth samples in the emulsion for three times, and drying at 90 ℃. One of the cloth samples was finished and then repeatedly washed with deionized water ten times.
And respectively carrying out oxygen index and vertical combustion tests on the two prepared cloth samples. The oxygen index of the cloth sample which is not washed with water is measured to reach 32.3 percent. The cloth sample is vertically combusted, no melting drips exist, the average damage length is 75mm, and in a 30s continuous vertical combustion test, the number of the melting drips is 20; after ten times of water washing, the cloth sample oxygen index is 33.8%. The cloth sample has no melting dripping during vertical combustion, the average damage length is 100mm, and the melting dripping number in a 30s continuous vertical combustion test is 28.
Comparative example 3 (use of conventional non-flame retardant polyester fabric)
A conventional polyester fabric (fiber size 150D/72f, about 2 dm)2) Adding into 80 deg.C hot water to remove oil.
Taking 1L of prepared Tris-HCl buffer solution with the pH value of 8.5 by using a beaker, weighing 2g of dopamine, adding the dopamine into the beaker, adding 4g of polyester fabric, covering the opening of the beaker with a preservative film, and reacting for 24 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, and drying the cloth sample. Taking 1L of fresh Tris-HCl buffer solution by using a beaker, adding 2g of 1-2 bis (1, 3 oxaborole) amyl ether (II), adding a cloth sample, covering the opening of the beaker with a preservative film, and reacting for 3 hours under mechanical stirring at 600 r/min.
And taking out the cloth sample after the reaction is finished, washing the cloth sample with deionized water for three times, drying the cloth sample, and testing the oxygen index and the vertical combustion. The oxygen index is measured to be 23.0%, the cloth sample has a melt dripping phenomenon during vertical combustion, the afterflame phenomenon is obvious, the average damage length is more than 150mm, the same cloth sample is further wound into a compact rod shape to be subjected to a 30-second continuous vertical combustion test, and the melt dripping can not be counted in 30-second combustion.
As can be seen from the above table, in general, as the amount of the anti-dripping agent increases, the oxygen index test results gradually decrease, which indicates that the flame retarding manner in which the phosphorus-based flame retardant partially promotes the heat removal by the dripping is suppressed by the addition of the anti-dripping agent, but this has to be sacrificed in order to achieve the cloth-like anti-dripping effect.
Examples 1, 2, and 3 show that increasing the chemical bonding of boron-based anti-drip agents helps to achieve the anti-drip effect when the amount of polydopamine on the fiber surface is kept constant, as shown by the reduction in the length of damage and the reduction in the number of drips during 30s of continuous combustion.
The comparison of examples 2 and 4 and examples 3 and 6 shows that the bonding capacity of a certain amount of polydopamine on the surface of the fiber to boron-based anti-dripping agents (I/II) is limited, and when the amount of the polydopamine is increased, the surface of the fiber can be effectively bonded with more boron-based anti-dripping agents, so that the anti-dripping capacity is further improved.
The comparison of examples 4 and 5 and examples 6 and 7 shows that the anti-dripping effect (the damage length and the number of molten drops) is slightly reduced after a plurality of times of water washing, but the water washing durability is greatly improved compared with the conventional padding method in comparative example 2.
Examples 8 and 9 show that there is almost no great difference in the effect of the two boron-based anti-dropping agents.
Comparative example 3 shows, in comparison with examples 1 and 9, that the introduction of a simple boron-based anti-dripping agent results in a modified fabric which does not have effective anti-dripping and flame-retardant effects due to the lack of dehydration and carbonization of polyphosphoric acid formed by a phosphorus-based flame retardant at high temperatures. Therefore, the phosphorus flame retardant still plays an important role in flame retarding and anti-dripping after finishing.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification is characterized in that: comprises polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fiber as a raw material and polydopamine and boron-based anti-dripping agents attached to the surface of the polyester fabric by an after-finishing method.
2. The poly-dopamine surface-modified phosphorus-boron compound after-finishing anti-dripping polyester fabric according to claim 1, wherein the boron-based anti-dripping agent is a compound having the following structure:
3. the polydopamine-surface-modified phosphorus-boron compound after-finishing anti-dripping polyester fabric as claimed in claim 1, wherein the fiber specification of the polyester fabric is 75-300D, 48-144f, and the phosphorus content is 4500-7000 ppm.
4. A method for preparing the phosphorus-boron compound after-finishing anti-dripping polyester fabric based on polydopamine surface modification according to any one of claims 1 to 3, which is characterized by comprising the following steps:
1) adding an oil removing agent into hot water, and adding polyester fabric prepared by taking phosphorus-containing flame-retardant polyester fiber as a raw material into the hot water to remove oil;
2) drying the polyester fabric after oil removal, adding the polyester fabric into a Tris-HCl buffer solution, adding a dopamine monomer, stirring, and realizing self-polymerization coating of dopamine by using oxygen in the air as a catalyst to obtain a poly-dopamine surface modified polyester fabric;
3) adding the boron system anti-dripping agent into a Tris-HCl buffer solution, and uniformly stirring to obtain an after-finishing solution containing the boron system anti-dripping agent; dipping the polyester fabric obtained in the step 2) in the after-finishing liquid and stirring to carry out surface grafting reaction; and finally, taking out the polyester fabric, washing and drying to obtain a finished product.
5. The method according to claim 4, wherein in the step 1), the oil is removed by washing with water at 75 to 85 ℃.
6. The method according to claim 4, wherein in step 2), the concentration of dopamine monomer in Tris-HCl buffer is 1-4 g/L; the mass volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L.
7. The method according to claim 4 or 6, wherein the stirring time in step 2) is 24 to 72 hours.
8. The method according to claim 4, wherein the Tris-HCl buffer solution has a pH of 8.2 to 8.8 in step 2) and step 3).
9. The method according to claim 4, wherein in step 3), the concentration of the boron-based anti-dropping agent in Tris-HCl buffer is 1 to 6 g/L; the mass volume ratio of the polyester fabric to the Tris-HCl buffer solution is 2-5 g/1-2L.
10. The method according to claim 4 or 9, wherein in step 3), the stirring time is 2 to 4 hours.
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