CN116043529A - Flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric and preparation method thereof - Google Patents
Flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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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
- 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
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
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- 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
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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Abstract
The invention relates to the technical field of cotton fabric clothing, and discloses a flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric, wherein hydroxyethyl chitosan and carboxyl on the surface of graphene oxide undergo esterification reaction to obtain chitosan grafted graphene, a dialdehyde group phosphoramide compound contains two active aromatic aldehyde groups and can respectively react with amino modified cotton fabric and amino groups on side chains of chitosan in a Schiff base crosslinking manner, so that the chitosan grafted graphene is actively crosslinked to the surface of the cotton fabric through the dialdehyde group phosphoramide compound, the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is obtained, the phosphoramide compound is decomposed at high temperature to generate oxygen-containing phosphoric acid, the oxygen-containing phosphoric acid can be very strong in water absorption, chitosan is used as an expansion carbon source, the thermal cracking of chitosan is promoted, and the graphene oxide forms a stable carbon barrier layer on the surface of cotton fiber, so that good flame retardance and smoke suppression effects are achieved.
Description
Technical Field
The invention relates to the technical field of cotton fabric clothing, in particular to a flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric and a preparation method thereof.
Background
The cotton fabric has excellent heat preservation, dyeing property, hygroscopicity, air permeability and other excellent properties, is one of the most commonly used fabrics, has important application in the aspects of clothing fabrics, decorative fabrics and the like, is increasingly abundant, and is a hot research on modification of the cotton fabric in recent years, such as antistatic finishing, flame retardant finishing and the like, and can improve the properties of the cotton fabric, such as flame retardance and the like.
The chitosan is used as a biomass material, has good compatibility with cotton fibers, can be used as an expansion carbon source and compounded with a phosphorus flame retardant, has wide application prospect in the flame retardant aspect of a high polymer material, and is a two-dimensional carbon nanomaterial with excellent performance, and is widely applied in the cotton fabric finishing aspect, and the graphene has good application in the flame retardant field in recent years, and ethanol can be used for combining the chitosan, the graphene and the phosphorus flame retardant to carry out flame retardant finishing on cotton fabrics.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric and a preparation method thereof, and the flame retardant property of the cotton fabric is improved.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric comprises the following steps of:
(1) Adding cotton fabric into ethanol and deionized water solvent, stirring uniformly, adding 3-aminopropyl trimethoxy silane, heating to 35-60 ℃ for reaction for 1-3h, filtering, washing with ethanol and deionized water, and obtaining amino modified cotton fabric.
(2) Adding graphene oxide and hydroxyethyl chitosan into a dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 6-18h at 20-40 ℃, adding dilute acetic acid to adjust the pH of the solution to 4-5 after the reaction, stirring uniformly, centrifugally separating, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding amino modified cotton fabric and chitosan grafted graphene into ethanol and deionized water solvents, uniformly stirring, adding a dialdehyde phosphoramide compound, heating for crosslinking reaction, centrifuging after the reaction, and washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric.
Preferably, the mass ratio of graphene oxide, hydroxyethyl chitosan, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide in the step (2) is 2-15:100:0.6-5:0.5-6.5.
Preferably, in the step (3), the mass ratio of the amino modified cotton fabric, the chitosan grafted graphene and the dialdehyde phosphoramide compound is 100:3-10:1.2-5.
Preferably, the dialdehyde phosphoramide compound in step (3) has the formula C 20 H 17 N 2 O 4 P, the structural formula is
Preferably, the temperature of the crosslinking reaction in the step (3) is 35-60 ℃ and the reaction time is 3-10h.
(III) beneficial technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is prepared by carrying out surface modification on cotton fabric by 3-aminopropyl trimethoxy silane to obtain amino modified cotton fabric, esterifying carboxyl groups on the surface of hydroxyethyl chitosan and graphene oxide in a catalytic system of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide to obtain chitosan grafted graphene, wherein a dialdehyde phosphoramide compound contains two active aromatic aldehyde groups and can respectively carry out Schiff base crosslinking reaction with amino groups on the side chains of the amino modified cotton fabric and amino groups on the side chains of chitosan, so that the chitosan grafted graphene is actively crosslinked to the surface of the cotton fabric by the dialdehyde phosphoramide compound, the graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric with flame retardance is obtained, the phosphorus amide compound is decomposed at high temperature to generate oxygen-containing phosphoric acid, so that the oxygen-containing phosphoric acid can be very strong in water absorption, chitosan is used as an expansion carbon source to promote thermal cracking carbonization of chitosan, and graphene oxide forms a stable carbon barrier layer on the surface of cotton fiber, so that the flame retardance and smoke suppression effects are very good, the cotton fabric is excellent in flame retardance finishing effect, the phosphorus flame retardant dialdehyde-phosphorus amide compound is added in examples 1-5, the graphene-chitosan and the cotton fabric are crosslinked and grafted, the good flame retardance is achieved, the dialdehyde-phosphorus amide compound is not added in comparative examples, and only the cotton fabric and the chitosan-graphene are physically blended, so that the flame retardance is poor.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: the preparation method of the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric comprises the following steps of:
(1) Adding cotton fabric into ethanol and deionized water solvent, stirring uniformly, adding 3-aminopropyl trimethoxy silane, heating to 35-60 ℃ for reaction for 1-3h, filtering, washing with ethanol and deionized water, and obtaining amino modified cotton fabric.
(2) Adding graphene oxide and hydroxyethyl chitosan into a dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 6-18 hours at 20-40 ℃, wherein the mass ratio of the graphene oxide to the hydroxyethyl chitosan to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide is 2-15:100:0.6-5:0.5-6.5, adding dilute acetic acid to adjust the pH of the solution to 4-5 after the reaction, stirring uniformly, centrifugally separating, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding amino modified cotton fabric and chitosan grafted graphene into ethanol and deionized water solvent, stirring uniformly, and adding dialdehyde phosphoramide compound (C) 20 H 17 N 2 O 4 And P), wherein the mass ratio of the amino modified cotton fabric to the chitosan grafted graphene to the dialdehyde phosphoramide compound is 100:3-10:1.2-5, heating to 35-60 ℃, carrying out a crosslinking reaction for 3-10h, centrifuging after the reaction, and washing the product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric.
The flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is placed in a JAY horizontal and vertical combustion tester for supporting a slice with the specification of 5cm multiplied by 5cm, and the fire grade is tested according to the experimental standard of UL94 method.
The GB/T17591-2006 is used as a test standard for testing the flame retardant property, the graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric with the flame retardant property is placed in a cone calorimeter, the heating rate is 10 ℃/min, the maximum test temperature is 800 ℃, and the peak value of the combustion heat release rate is tested.
Example 1
(1) Adding 0.5g of cotton fabric into 100mL of ethanol and 10mL of deionized water solvent, uniformly stirring, then adding 0.05g of 3-aminopropyl trimethoxysilane, heating to 35 ℃ for reaction for 1h, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 0.02g of graphene oxide and 1g of hydroxyethyl chitosan into 50mL of dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 0.006g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 0.005g of N-hydroxysuccinimide, reacting for 6 hours at 20 ℃, adding dilute acetic acid to adjust the pH of the solution to 4 after the reaction, stirring uniformly, centrifuging, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding 1g of amino modified cotton fabric and 0.03g of chitosan grafted graphene into ethanol and deionized water solvent, uniformly stirring, and adding 0.012g of dialdehyde phosphoramide compound (C 20 H 17 N 2 O 4 P) heating to 35 ℃ for crosslinking reaction for 3h, centrifugally separating after the reaction, washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric, wherein the UL94 fireproof grade is V-1, and the peak value of the combustion heat release rate is 48.6kWm -2 。
Example 2
(1) Adding 0.5g of cotton fabric into 150mL of ethanol and 15mL of deionized water solvent, uniformly stirring, then adding 0.08g of 3-aminopropyl trimethoxysilane, heating to 40 ℃ for reaction for 1h, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 0.05g of graphene oxide and 1g of hydroxyethyl chitosan into 100mL of dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 0.015g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 0.012g of N-hydroxysuccinimide, reacting for 18h at 30 ℃, adding dilute acetic acid to adjust the pH of the solution to 4 after the reaction, stirring uniformly, centrifuging, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding 1g of amino modified cotton fabric and 0.06g of chitosan grafted graphene into ethanol and deionized water solvent, uniformly stirring, and adding 0.03g of dialdehyde phosphoramide compound (C) 20 H 17 N 2 O 4 P) heating to 40 ℃, carrying out crosslinking reaction for 3h, centrifuging and separating after the reaction, and washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric, wherein the UL94 fireproof grade is V-0, and the peak value of the combustion heat release rate is 42.6kWm -2 。
Example 3
(1) Adding 0.5g of cotton fabric into 200mL of ethanol and 20mL of deionized water solvent, uniformly stirring, then adding 0.1g of 3-aminopropyl trimethoxysilane, heating to 40 ℃ for reaction for 2 hours, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 0.08g of graphene oxide and 1g of hydroxyethyl chitosan into 150mL of dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 0.03g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 0.025g of N-hydroxysuccinimide, reacting for 12 hours at 30 ℃, adding dilute acetic acid to adjust the pH of the solution to 5 after the reaction, stirring uniformly, centrifuging, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding 1g of amino modified cotton fabric and 0.7g of chitosan grafted graphene into ethanol and deionized water solvent, uniformly stirring, and then adding 0.035g of dialdehyde group phosphoramide compound (C) 20 H 17 N 2 O 4 P) heating to 40 ℃, carrying out crosslinking reaction for 8 hours, centrifuging and separating after the reaction, washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric, wherein the UL94 fireproof grade is V-0, and the peak value of the combustion heat release rate is 37.0kWm -2 。
Example 4
(1) Adding 0.5g of cotton fabric into 250mL of ethanol and 25mL of deionized water solvent, uniformly stirring, then adding 0.12g of 3-aminopropyl trimethoxysilane, heating to 40 ℃ for reaction for 2 hours, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 0.12g of graphene oxide and 1g of hydroxyethyl chitosan into 200mL of dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 0.04g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 0.035g of N-hydroxysuccinimide, reacting for 12 hours at 30 ℃, adding dilute acetic acid to adjust the pH of the solution to 4 after the reaction, stirring uniformly, centrifuging, washing the product by distilled water and ethanol, and obtaining the chitosan grafted graphene.
(3) Adding 1g of amino modified cotton fabric and 0.08g of chitosan grafted graphene into ethanol and deionized water solvent, uniformly stirring, and adding 0.04g of dialdehyde phosphoramide compound (C) 20 H 17 N 2 O 4 P) heating to 50 ℃ for crosslinking reaction for 8 hours, centrifugally separating after the reaction, washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric, wherein the UL94 fireproof grade is V-0, and the peak value of the combustion heat release rate is 44.1kWm -2 。
Example 5
(1) Adding 0.5g of cotton fabric into 300mL of ethanol and 30mL of deionized water solvent, uniformly stirring, then adding 0.15g of 3-aminopropyl trimethoxysilane, heating to 60 ℃ for reaction for 3 hours, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 0.15g of graphene oxide and 1g of hydroxyethyl chitosan into 300mL of dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 0.05g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 0.045g of N-hydroxysuccinimide, reacting for 8 hours at 40 ℃, adding dilute acetic acid to adjust the pH of the solution to 5 after the reaction, stirring uniformly, centrifuging, and washing the product by distilled water and ethanol to obtain the chitosan grafted graphene.
(3) Adding 1g of amino modified cotton fabric and 0.1g of chitosan grafted graphene into ethanol and deionized water solvent, uniformly stirring, and adding 0.05g of dialdehyde phosphoramide compound (C) 20 H 17 N 2 O 4 P) heating to 60 DEG CCrosslinking reaction for 10h, centrifugal separation after reaction, washing the product with ethanol to obtain the graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric with flame retardance, UL94 fire resistance grade of V-0 and combustion heat release rate peak value of 45.2kWm -2 。
Comparative example 1
(1) Adding 0.5g of cotton fabric into 200mL of ethanol and 15mL of deionized water solvent, uniformly stirring, then adding 0.1g of 3-aminopropyl trimethoxysilane, heating to 40 ℃ for reaction for 1h, filtering, and washing with ethanol and deionized water to obtain the amino modified cotton fabric.
(2) Adding 1g of amino modified cotton fabric and 0.5g of chitosan grafted graphene into ethanol and deionized water solvent, stirring and mixing uniformly, centrifuging after reaction, and washing a product with ethanol to obtain the graphene-chitosan loaded cotton fabric, wherein the UL94 fireproof grade is V-2, and the peak combustion heat release rate is 54.8kW m -2 。
Claims (5)
1. A flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is characterized in that: the preparation method of the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric comprises the following steps of:
(1) Adding cotton fabric into ethanol and deionized water solvent, stirring uniformly, then adding 3-aminopropyl trimethoxy silane, heating to 35-60 ℃ for reaction for 1-3h, filtering, washing with ethanol and deionized water to obtain amino modified cotton fabric;
(2) Adding graphene oxide and hydroxyethyl chitosan into a dimethylformamide solvent, uniformly dispersing by ultrasonic, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, reacting for 6-18 hours at 20-40 ℃, adding dilute acetic acid to adjust the pH of the solution to 4-5 after the reaction, stirring uniformly, centrifugally separating, and washing the product by distilled water and ethanol to obtain chitosan grafted graphene;
(3) Adding amino modified cotton fabric and chitosan grafted graphene into ethanol and deionized water solvents, uniformly stirring, adding a dialdehyde phosphoramide compound, heating for crosslinking reaction, centrifuging after the reaction, and washing a product with ethanol to obtain the flame-retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric.
2. The flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric according to claim 1, wherein the flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is characterized in that: the mass ratio of graphene oxide, hydroxyethyl chitosan, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide in the step (2) is 2-15:100:0.6-5:0.5-6.5.
3. The flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric according to claim 1, wherein the flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is characterized in that: in the step (3), the mass ratio of the amino modified cotton fabric to the chitosan grafted graphene to the dialdehyde phosphoramide compound is 100:3-10:1.2-5.
4. The flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric according to claim 1, wherein the flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is characterized in that: the molecular formula of the dialdehyde phosphoramide compound in the step (3) is C 20 H 17 N 2 O 4 P, the structural formula is
5. The flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric according to claim 1, wherein the flame retardant graphene-phosphorus-containing chitosan crosslinked grafted cotton fabric is characterized in that: the temperature of the crosslinking reaction in the step (3) is 35-60 ℃ and the reaction time is 3-10h.
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