CN112281492A - Anti-aging textile fabric and preparation method thereof - Google Patents
Anti-aging textile fabric and preparation method thereof Download PDFInfo
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- CN112281492A CN112281492A CN202011223240.XA CN202011223240A CN112281492A CN 112281492 A CN112281492 A CN 112281492A CN 202011223240 A CN202011223240 A CN 202011223240A CN 112281492 A CN112281492 A CN 112281492A
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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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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/14—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with hydrogen or carbon atoms directly attached to at least one ring carbon atom
- C07D251/24—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with hydrogen or carbon atoms directly attached to at least one ring carbon atom to three ring carbon atoms
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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- 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
- D06M13/10—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 oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
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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
- D06M13/322—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
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
- D06M13/358—Triazines
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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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- 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
- D06M15/55—Epoxy resins
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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
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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Abstract
The invention discloses an anti-aging textile fabric and a preparation method thereof, the anti-aging textile fabric is prepared from terylene gray cloth, a first impregnation liquid and a second impregnation liquid, a water-resistant agent is prepared in the first impregnation liquid, the water-resistant agent is prepared by the reaction of amino in chitosan molecules and carboxyl on carboxymethyl chitosan, so that the chitosan molecules are connected with modified nano titanium dioxide to prepare the water-resistant agent, a short fluorocarbon chain monomer on the surface of the water-resistant agent has good hydrophobicity, an anti-aging agent is prepared in the second impregnation liquid, the ortho-position of the carbonyl of the anti-aging agent contains hydroxyl to form intramolecular hydrogen bonds, so that the anti-aging agent has a stable conjugated structure, can effectively absorb ultraviolet rays, the intramolecular hydrogen bonds are broken after the ultraviolet rays are absorbed, hydrogen bond rings are opened to form ionic compounds, the structure is unstable, and redundant energy can be released in harmless heat energy in order to achieve a stable state, and then the hydrogen bonds are recovered, and the textile fabric is protected from photochemical reaction.
Description
Technical Field
The invention relates to the technical field of fabric preparation, in particular to an anti-aging textile fabric and a preparation method thereof.
Background
Polyester fiber, commonly called as 'polyester', is a synthetic fiber obtained by spinning polyester formed by polycondensation of organic dibasic acid and dihydric alcohol, called as PET fiber for short, belongs to a high molecular compound, is invented in 1941 and is the first major variety of the current synthetic fiber, the polyester fiber has the greatest advantages of good crease resistance and shape retention, higher strength and elasticity recovery capability, firmness and durability, crease resistance, no ironing, no hair sticking, and the like, so that the polyester fiber is widely applied to clothes, decorations, textiles and the like, but with the improvement of world science and technology and the development of economy, the requirements of people on the performance and the functions of the polyester fiber are higher and higher. More and more researches on terylene materials and process methods
After the existing polyester textile fabric is used for a long time, the fabric can age, so that the service life of the fabric is shortened, an anti-aging agent can be added into part of the fabric in the preparation process, but after the fabric is washed for many times, the anti-aging agent in the fabric runs off, so that the anti-aging performance of the fabric is reduced.
Disclosure of Invention
The invention aims to provide an anti-aging textile fabric and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
after the existing textile fabric is washed for a plurality of times, the anti-aging agent in the fabric runs off, so that the anti-aging performance of the fabric is reduced.
The purpose of the invention can be realized by the following technical scheme:
an anti-aging textile fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 20-24h at the temperature of 25-30 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and padding for 5-8h at the temperature of 120-150 ℃ to obtain first padded polyester gray cloth;
step S3: padding the first padding terylene grey cloth prepared in the step S2 in a second impregnation liquid, padding for 5-8h at the temperature of 120-150 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
Further, the concentration of the dopamine solution in step S1 is 0.5g/L, the first impregnation liquid is a mixture of bisphenol a epoxy resin, 2-octanone, and a water-resistant agent at a mass ratio of 1.2:5:1, and the second impregnation liquid is a mixture of bisphenol a epoxy resin, 2-octanone, and an aging-resistant agent at a mass ratio of 2:5: 1.
Further, the water-resistant agent is prepared by the following steps:
step A1: adding tetrabutyl titanate and absolute ethyl alcohol into a reaction kettle, stirring and dropwise adding glacial acetic acid solution at the rotation speed of 120-130r/min and the temperature of 50-55 ℃, wherein the dropwise adding speed is 0.05mL/s, after the dropwise adding is finished, adding polyethylene glycol, adjusting the pH of the reaction solution to 2-3, reacting for 15-20min, adding trifluoropropylmethyl cyclotrisiloxane and deionized water, reacting for 10-15min at the frequency of 3-5MHz and the temperature of 80-85 ℃, filtering to remove filtrate, and drying a filter cake to obtain modified nano titanium dioxide;
step A2: and (2) adding carboxymethyl chitosan and a hydrochloric acid solution into a reaction kettle, stirring until the chitosan is dissolved, adding the modified nano titanium dioxide and the 1-hydroxybenzotriazole prepared in the step A1, carrying out ultrasonic treatment for 30-50min under the conditions that the frequency is 5-8MHz and the temperature is 35-40 ℃, filtering to remove filtrate, and drying a filter cake to obtain the water-resistant agent.
Further, the dosage ratio of tetrabutyl titanate, anhydrous ethanol, glacial acetic acid and polyethylene glycol in the step A1 is 10mL:20mL:25mL:1g, the glacial acetic acid solution is formed by mixing anhydrous ethanol and glacial acetic acid according to the volume ratio of 2.5:2, the dosage of trifluoropropylmethyl cyclotrisiloxane is 3-5% of the mass of tetrabutyl titanate, the dosage mass ratio of carboxymethyl chitosan to nano titanium dioxide in the step A2 is 8:1-1.5, and the dosage of 1-hydroxy benzotriazole is 30-35% of the mass of modified nano titanium dioxide.
Further, the aging resistant agent is prepared by the following steps:
step B1: dissolving cyanuric chloride into ether to prepare cyanuric chloride solution, adding resorcinol and ether into a reaction kettle, stirring at the rotation speed of 120-150r/min and at the temperature of 40-50 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the cyanuric chloride solution, and reacting for 8-10h to prepare an intermediate 1;
the reaction process is as follows:
step B2: dissolving 2- (2-hydroxy-5-benzyl) benzotriazole in tetrahydrofuran, adding chloroacetyl chloride, reacting for 3-5h at the rotation speed of 200-300r/min and the temperature of 35-40 ℃, adding anhydrous aluminum trichloride and triethylamine, reacting for 3-5h at the rotation speed of 500-800r/min and the temperature of 120-125 ℃ to obtain an intermediate 2, dissolving the intermediate 2 in tetrahydrofuran, adding step B1 to obtain an intermediate 1, and reacting for 2-3h at the temperature of 25-30 ℃ to obtain an intermediate 3;
the reaction process is as follows:
step B3: adding 3-nitrophenol, 2-nitro-4-hydroxybenzoic acid, anhydrous zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, stirring uniformly at the rotation speed of 120-plus 150r/min, heating to the temperature of 75-80 ℃, reacting for 2-3h, adding deionized water, standing for 20-30min, cooling to the temperature of 15-20 ℃, filtering to remove filtrate to obtain an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, and reacting for 3-5h at the temperature of 85-90 ℃ to obtain an intermediate 5;
the reaction process is as follows:
step B4: adding the intermediate 5, iron powder and ethanol into a reaction kettle, performing reflux reaction at 80-85 ℃ for 3-5h, adding hydrochloric acid solution for 20min, continuing to react for 5-8h, and adjusting the pH value of the reaction solution to 7-8 to obtain an intermediate 6; adding the intermediate 6 and sulfolane into a reaction kettle, stirring at the rotation speed of 120-plus-150 r/min until the intermediate 6 is completely dissolved, heating to the temperature of 30-35 ℃, introducing phosgene, continuously stirring for 30-50min, heating to the temperature of 120-plus-150 ℃, continuously reacting for 2-3h, cooling to the temperature of 90-100 ℃, introducing nitrogen to remove phosgene, and preserving heat for 10-15min to obtain an intermediate 7;
the reaction process is as follows:
step B5: dissolving the intermediate 7 in medium tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished to obtain an intermediate 8, dissolving the intermediate 3 in tetrahydrofuran to obtain an intermediate 3 solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120-150r/min and the temperature of 80-90 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the intermediate 3 solution, reacting for 5-8h, adding the intermediate 8 and the anhydrous potassium manganese carbonate prepared in the step B4, introducing nitrogen for protection, and performing reflux reaction for 5-8h at the temperature of 80-90 ℃ to obtain the anti-aging agent.
The reaction process is as follows:
further, the molar ratio of the cyanuric chloride to the resorcinol in the step B1 is 1:2, the amount of anhydrous aluminum trichloride is 5-10% of the mass of the cyanuric chloride, the molar ratio of the 2- (2-hydroxy-5-benzyl) benzotriazole, the chloroacetyl chloride and the anhydrous aluminum trichloride in the step B2 is 1:1:1.2, the amount of triethylamine is 3-5% of the mass of the 2- (2-hydroxy-5-benzyl) benzotriazole, the molar ratio of the 3-nitrophenol, the 2-nitro-4-hydroxybenzoic acid, the anhydrous zinc chloride and the phosphorus oxychloride in the step B3 is 1.4:1:1.5:2, the molar ratio of the intermediate 4, the potassium carbonate and the dimethyl sulfate is 3:1:1, and the intermediate 5, the iron powder, the ethanol, the methanol and the methanol in the step B4 are mixed, and the mixture is obtained by mixing the reaction of the cyanuric chloride and the methanol, 2g of hydrochloric acid solution, 4.5g of hydrochloric acid solution, 60mL of hydrochloric acid solution and 10mL of ethanol, wherein the volume fraction of the ethanol is 90%, the hydrochloric acid solution is formed by mixing concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% in a volume ratio of 1:9, the using amount molar ratio of an intermediate 6 to phosgene is 1:1, the using amount molar ratio of an intermediate 7 to boron tribromide in the step B5 is 1g to 3mL, the using amount molar ratio of an intermediate 3, resorcinol and an intermediate 8 is 1:1:1, the using amount of anhydrous aluminum trichloride is 5-10% of the mass of the intermediate 3, and the using amount of anhydrous potassium manganese carbonate is 3-5% of the mass of the intermediate 8.
A preparation method of an anti-aging textile fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 20-24h at the temperature of 25-30 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and padding for 5-8h at the temperature of 120-150 ℃ to obtain first padded polyester gray cloth;
step S3: padding the first padding terylene grey cloth prepared in the step S2 in a second impregnation liquid, padding for 5-8h at the temperature of 120-150 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
The invention has the beneficial effects that: the invention discloses a water-proof agent in the process of preparing an anti-aging textile fabric, which is prepared by taking tetrabutyl titanate as a raw material, preparing nano titanium dioxide by a gel method, carrying out surface modification by trifluoropropyl methyl cyclotrisiloxane, further forming a hydrophobic film on the surface of the nano titanium dioxide, further reacting amino in chitosan molecules with carboxyl on carboxymethyl chitosan under the action of 1-hydroxy benzotriazole, so that the chitosan molecules are connected with the modified nano titanium dioxide, preparing the water-proof agent, wherein a short fluorocarbon chain monomer on the surface of the water-proof agent has good hydrophobicity, preparing an anti-aging agent, reacting cyanuric chloride with m-diphenol, preparing an intermediate 1 by controlling the temperature, reacting 2- (2-hydroxy-5-benzyl) benzotriazole with chloroacetyl chloride, and then carrying out Fries rearrangement to prepare an intermediate 2, the intermediate 2 reacts with the intermediate 1 to prepare an intermediate 3, 3-nitrophenol reacts with 2-nitro-4-hydroxybenzoic acid to prepare an intermediate 4, the intermediate 4 is subjected to hydroxyl protection to prepare an intermediate 5, the intermediate 5 is reduced to convert nitro into amino to prepare an intermediate 6, one amino on the intermediate 6 is converted into isocyanate by controlling the light amount to prepare an intermediate 7, the intermediate 7 is subjected to deprotection to prepare an intermediate 8, the intermediate 3 further reacts with m-diphenol and reacts with the intermediate 8 to prepare the aging resistant agent, the ortho position of the aging resistant carbonyl contains hydroxyl to form an intramolecular hydrogen bond, so that the aging resistant carbonyl has a stable conjugated structure, can effectively absorb ultraviolet rays, the intramolecular hydrogen bond is destroyed after the ultraviolet rays are absorbed, and a hydrogen bond ring is opened to form an ionic compound, the structure is unstable, redundant energy can be released by harmless heat energy to achieve a stable state, so that hydrogen bonds are restored, the textile fabric is protected from photochemical reaction, the existing dopamine solution of the polyester gray cloth is treated to form a layer of polydopamine on the surface of the polyester gray cloth, the polyester gray cloth is soaked in a first enhancing solution, two epoxy groups of epoxy resin in the first enhancing solution are subjected to ring opening reaction, one epoxy group is subjected to ring opening reaction with hydroxyl groups on the polydopamine on the surface of the polyester gray cloth, the other epoxy group is subjected to reaction with hydroxyl groups on a water-resistant agent and then is soaked in a second soaking solution, the hydroxyl groups on the residual polydopamine on the surface of the polyester gray cloth are subjected to ring opening reaction with one epoxy group in the epoxy resin, the other epoxy group is subjected to ring opening reaction with an anti-aging agent, so that a water-resistant layer and an anti-aging layer are formed on the surface of the polyester gray cloth, and the effects of the water-resistant layer and the anti-, the service life of the textile fabric is prolonged.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An anti-aging textile fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 20 hours at the temperature of 25 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and performing padding for 5 hours at the temperature of 120 ℃ to obtain first padded polyester gray cloth;
step S3: and padding the first padded polyester gray cloth prepared in the step S2 in a second impregnation liquid, padding for 5 hours at the temperature of 120 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
The water-resistant agent is prepared by the following steps:
step A1: adding tetrabutyl titanate and absolute ethyl alcohol into a reaction kettle, stirring and dropwise adding glacial acetic acid solution at the rotation speed of 120r/min and the temperature of 50 ℃, adding polyethylene glycol and regulating the pH of a reaction solution to be 2 after dropwise adding, reacting for 15min, adding trifluoropropylmethyl cyclotrisiloxane and deionized water, reacting for 10min at the frequency of 3MHz and the temperature of 80 ℃, filtering to remove filtrate, and drying a filter cake to obtain modified nano titanium dioxide;
step A2: and (2) adding carboxymethyl chitosan and a hydrochloric acid solution into a reaction kettle, stirring until the chitosan is dissolved, adding the modified nano titanium dioxide and the 1-hydroxy benzotriazole prepared in the step A1, carrying out ultrasonic treatment for 30min under the conditions of the frequency of 5MHz and the temperature of 35 ℃, filtering to remove filtrate, and drying a filter cake to obtain the water-resistant agent.
The aging resistant agent is prepared by the following steps:
step B1: dissolving cyanuric chloride in diethyl ether to prepare cyanuric chloride solution, adding m-diphenol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120r/min and the temperature of 40 ℃ until the m-diphenol is completely dissolved, adding anhydrous aluminum trichloride and the cyanuric chloride solution, and reacting for 8 hours to prepare an intermediate 1;
step B2: dissolving 2- (2-hydroxy-5-benzyl) benzotriazole in tetrahydrofuran, adding chloroacetyl chloride, reacting for 3h at 35 ℃ at a rotation speed of 200r/min, adding anhydrous aluminum trichloride and triethylamine, reacting for 3h at 120 ℃ at a rotation speed of 500r/min to obtain an intermediate 2, dissolving the intermediate 2 in tetrahydrofuran, adding step B1 to obtain an intermediate 1, and reacting for 2h at 25 ℃ to obtain an intermediate 3;
step B3: adding 3-nitrophenol, 2-nitro-4-hydroxybenzoic acid, anhydrous zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, stirring uniformly at the rotation speed of 120r/min, heating to 75 ℃, reacting for 2 hours, adding deionized water, standing for 20 minutes, cooling to 15 ℃, filtering to remove filtrate, preparing an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, and reacting for 3 hours at the temperature of 85 ℃ to prepare an intermediate 5;
step B4: adding the intermediate 5, iron powder and ethanol into a reaction kettle, performing reflux reaction for 3 hours at the temperature of 80 ℃, adding a hydrochloric acid solution for 20 minutes, continuing to react for 5 hours, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 6; adding the intermediate 6 and sulfolane into a reaction kettle, stirring at the rotation speed of 120r/min until the intermediate 6 is completely dissolved, heating to the temperature of 30 ℃, introducing phosgene, continuously stirring for 30min, heating to the temperature of 120 ℃, continuously reacting for 2h, cooling to the temperature of 90 ℃, introducing nitrogen to remove phosgene, and preserving heat for 10min to obtain an intermediate 7;
step B5: dissolving the intermediate 7 in medium tetrahydrofuran, adding boron tribromide at the temperature of-70 ℃, reacting for 10 hours at the temperature of 25 ℃ after the addition is finished to obtain an intermediate 8, dissolving the intermediate 3 in tetrahydrofuran to obtain an intermediate 3 solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120r/min and the temperature of 80 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the intermediate 3 solution, reacting for 5 hours, adding the intermediate 8 and the anhydrous potassium manganese carbonate prepared in the step B4, introducing nitrogen for protection, and performing reflux reaction for 5 hours at the temperature of 80 ℃ to obtain the anti-aging agent.
Example 2
An anti-aging textile fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 24 hours at the temperature of 25 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and performing padding for 8 hours at the temperature of 120 ℃ to obtain first padded polyester gray cloth;
step S3: and padding the first padded polyester gray cloth prepared in the step S2 in a second impregnation liquid, padding for 8 hours at the temperature of 120 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
The water-resistant agent is prepared by the following steps:
step A1: adding tetrabutyl titanate and absolute ethyl alcohol into a reaction kettle, stirring and dropwise adding glacial acetic acid solution at the rotation speed of 120r/min and the temperature of 55 ℃, adding polyethylene glycol and regulating the pH of a reaction solution to be 2 after dropwise adding, reacting for 20min, adding trifluoropropylmethyl cyclotrisiloxane and deionized water, reacting for 10min at the frequency of 3MHz and the temperature of 85 ℃, filtering to remove filtrate, and drying a filter cake to obtain modified nano titanium dioxide;
step A2: and (2) adding carboxymethyl chitosan and a hydrochloric acid solution into a reaction kettle, stirring until the chitosan is dissolved, adding the modified nano titanium dioxide and the 1-hydroxy benzotriazole prepared in the step A1, carrying out ultrasonic treatment for 50min under the conditions of the frequency of 8MHz and the temperature of 35 ℃, filtering to remove filtrate, and drying a filter cake to obtain the water-resistant agent.
The aging resistant agent is prepared by the following steps:
step B1: dissolving cyanuric chloride in diethyl ether to prepare cyanuric chloride solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120r/min and the temperature of 50 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the cyanuric chloride solution, and reacting for 8 hours to prepare an intermediate 1;
step B2: dissolving 2- (2-hydroxy-5-benzyl) benzotriazole in tetrahydrofuran, adding chloroacetyl chloride, reacting for 5 hours at the temperature of 35 ℃ at the rotation speed of 300r/min, adding anhydrous aluminum trichloride and triethylamine, reacting for 3 hours at the rotation speed of 500r/min at the temperature of 125 ℃ to obtain an intermediate 2, dissolving the intermediate 2 in tetrahydrofuran, adding step B1 to obtain an intermediate 1, and reacting for 2 hours at the temperature of 30 ℃ to obtain an intermediate 3;
step B3: adding 3-nitrophenol, 2-nitro-4-hydroxybenzoic acid, anhydrous zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, stirring uniformly at the rotation speed of 150r/min, heating to 75 ℃, reacting for 3 hours, adding deionized water, standing for 20 minutes, cooling to 20 ℃, filtering to remove filtrate, preparing an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, and reacting for 5 hours at the temperature of 85 ℃ to prepare an intermediate 5;
step B4: adding the intermediate 5, iron powder and ethanol into a reaction kettle, performing reflux reaction for 5 hours at the temperature of 80 ℃, adding a hydrochloric acid solution for 20min, continuing to react for 5 hours, and adjusting the pH value of a reaction solution to 8 to obtain an intermediate 6; adding the intermediate 6 and sulfolane into a reaction kettle, stirring at the rotation speed of 120r/min until the intermediate 6 is completely dissolved, heating to 35 ℃, introducing phosgene, continuously stirring for 30min, heating to 50 ℃, continuously reacting for 2h, cooling to 100 ℃, introducing nitrogen to remove phosgene, and preserving heat for 10min to obtain an intermediate 7;
step B5: dissolving the intermediate 7 in medium tetrahydrofuran, adding boron tribromide at the temperature of minus 80 ℃, reacting for 15 hours at the temperature of 25 ℃ after the addition is finished to obtain an intermediate 8, dissolving the intermediate 3 in tetrahydrofuran to obtain an intermediate 3 solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120r/min and the temperature of 90 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the intermediate 3 solution, reacting for 5 hours, adding the intermediate 8 and the anhydrous potassium manganese carbonate prepared in the step B4, introducing nitrogen for protection, and performing reflux reaction for 5 hours at the temperature of 90 ℃ to obtain the anti-aging agent.
Example 3
An anti-aging textile fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 24 hours at the temperature of 30 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and performing padding for 8 hours at the temperature of 150 ℃ to obtain first padded polyester gray cloth;
step S3: and padding the first padded polyester gray cloth prepared in the step S2 in a second impregnation liquid, padding for 8 hours at the temperature of 150 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
The water-resistant agent is prepared by the following steps:
step A1: adding tetrabutyl titanate and absolute ethyl alcohol into a reaction kettle, stirring and dropwise adding glacial acetic acid solution at the rotation speed of 130r/min and the temperature of 55 ℃, adding polyethylene glycol and regulating the pH of a reaction solution to 3 after dropwise adding, reacting for 20min, adding trifluoropropylmethyl cyclotrisiloxane and deionized water, reacting for 15min at the frequency of 5MHz and the temperature of 85 ℃, filtering to remove filtrate, and drying a filter cake to obtain modified nano titanium dioxide;
step A2: and (2) adding carboxymethyl chitosan and a hydrochloric acid solution into a reaction kettle, stirring until the chitosan is dissolved, adding the modified nano titanium dioxide and the 1-hydroxy benzotriazole prepared in the step A1, carrying out ultrasonic treatment for 50min under the conditions of the frequency of 8MHz and the temperature of 40 ℃, filtering to remove filtrate, and drying a filter cake to obtain the water-resistant agent.
The aging resistant agent is prepared by the following steps:
step B1: dissolving cyanuric chloride in diethyl ether to prepare cyanuric chloride solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 150r/min and the temperature of 50 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the cyanuric chloride solution, and reacting for 10 hours to prepare an intermediate 1;
step B2: dissolving 2- (2-hydroxy-5-benzyl) benzotriazole in tetrahydrofuran, adding chloroacetyl chloride, reacting for 5 hours at 40 ℃ at the rotation speed of 300r/min, adding anhydrous aluminum trichloride and triethylamine, reacting for 5 hours at 125 ℃ at the rotation speed of 800r/min to obtain an intermediate 2, dissolving the intermediate 2 in tetrahydrofuran, adding step B1 to obtain an intermediate 1, and reacting for 3 hours at 30 ℃ to obtain an intermediate 3;
step B3: adding 3-nitrophenol, 2-nitro-4-hydroxybenzoic acid, anhydrous zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, stirring uniformly at the rotation speed of 150r/min, heating to 80 ℃, reacting for 3 hours, adding deionized water, standing for 30 minutes, cooling to 20 ℃, filtering to remove filtrate, preparing an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, and reacting for 5 hours at the temperature of 90 ℃ to prepare an intermediate 5;
step B4: adding the intermediate 5, iron powder and ethanol into a reaction kettle, performing reflux reaction for 5 hours at the temperature of 85 ℃, adding a hydrochloric acid solution for 20 minutes, continuing to react for 8 hours, and adjusting the pH value of the reaction solution to 8 to obtain an intermediate 6; adding the intermediate 6 and sulfolane into a reaction kettle, stirring at the rotation speed of 150r/min until the intermediate 6 is completely dissolved, heating to 35 ℃, introducing phosgene, continuously stirring for 50min, heating to 150 ℃, continuously reacting for 3h, cooling to 100 ℃, introducing nitrogen to remove phosgene, and keeping the temperature for 15min to obtain an intermediate 7;
step B5: dissolving the intermediate 7 in medium tetrahydrofuran, adding boron tribromide at the temperature of 80 ℃ below zero, reacting for 15 hours at the temperature of 30 ℃ after the addition is finished to obtain an intermediate 8, dissolving the intermediate 3 in tetrahydrofuran to obtain an intermediate 3 solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 150r/min and the temperature of 90 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the intermediate 3 solution, reacting for 8 hours, adding the intermediate 8 prepared in the step B4 and anhydrous potassium manganese carbonate, introducing nitrogen for protection, and performing reflux reaction for 8 hours at the temperature of 90 ℃ to obtain the anti-aging agent.
Comparative example
The comparative example is a common textile fabric in the market;
aging resistance: the textile fabrics prepared in examples 1-3 and comparative example were used at a wavelength of 340nm and a pre-irradiation degree of 0.68W/m2The temperature of the blackboard is 60 ℃, and the condensation temperature is 60 ℃; a single cycle process; illuminating for 3h, and blowing for 10 min; the cycle is repeated continuously for a total experimental time 168; after aging, testing tensile strength, tear strength, elongation at break;
TABLE 1
From the above table 1, it can be seen that the tensile strength, the elongation at break and the tear strength of the textile fabrics prepared in examples 1 to 3 are not reduced after aging, the tensile strength, the elongation at break and the tear strength of the textile fabrics prepared in comparative examples are reduced after aging, the tensile strength, the elongation at break and the tear strength of the textile fabrics prepared in examples 1 to 3 are not reduced after 50 times of water washing, and the tensile strength, the elongation at break and the tear strength of the textile fabrics prepared in comparative examples are reduced after 50 times of water washing, so that the surface of the invention has good aging resistance and water resistance.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. An ageing-resistant textile fabric is characterized in that: the polyester fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 20-24h at the temperature of 25-30 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and padding for 5-8h at the temperature of 120-150 ℃ to obtain first padded polyester gray cloth;
step S3: padding the first padding terylene grey cloth prepared in the step S2 in a second impregnation liquid, padding for 5-8h at the temperature of 120-150 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
2. The aging-resistant textile fabric as claimed in claim 1, wherein: the concentration of the dopamine solution in the step S1 is 0.5g/L, the first impregnation liquid is a mixture of bisphenol a epoxy resin, 2-octanone and a water-resistant agent in a mass ratio of 1.2:5:1, and the second impregnation liquid is a mixture of bisphenol a epoxy resin, 2-octanone and an aging-resistant agent in a mass ratio of 2:5: 1.
3. An ageing-resistant textile fabric as claimed in claim 2, wherein: the water-resistant agent is prepared by the following steps:
step A1: adding tetrabutyl titanate and absolute ethyl alcohol into a reaction kettle, stirring and dropwise adding glacial acetic acid solution at the rotation speed of 120-130r/min and the temperature of 50-55 ℃, wherein the dropwise adding speed is 0.05mL/s, after the dropwise adding is finished, adding polyethylene glycol, adjusting the pH of the reaction solution to 2-3, reacting for 15-20min, adding trifluoropropylmethyl cyclotrisiloxane and deionized water, reacting for 10-15min at the frequency of 3-5MHz and the temperature of 80-85 ℃, filtering to remove filtrate, and drying a filter cake to obtain modified nano titanium dioxide;
step A2: and (2) adding carboxymethyl chitosan and a hydrochloric acid solution into a reaction kettle, stirring until the chitosan is dissolved, adding the modified nano titanium dioxide and the 1-hydroxybenzotriazole prepared in the step A1, carrying out ultrasonic treatment for 30-50min under the conditions that the frequency is 5-8MHz and the temperature is 35-40 ℃, filtering to remove filtrate, and drying a filter cake to obtain the water-resistant agent.
4. An ageing-resistant textile fabric as claimed in claim 3, wherein: the dosage ratio of the tetrabutyl titanate, the absolute ethyl alcohol, the glacial acetic acid and the polyethylene glycol in the step A1 is 10mL:20mL:25mL:1g, the glacial acetic acid solution is the mixture of the absolute ethyl alcohol and the glacial acetic acid according to the volume ratio of 2.5:2, the dosage of the trifluoropropyl methyl cyclotrisiloxane is 3-5% of the mass of the tetrabutyl titanate, the dosage mass ratio of the carboxymethyl chitosan and the nano titanium dioxide in the step A2 is 8:1-1.5, and the dosage of the 1-hydroxy benzotriazole is 30-35% of the mass of the modified nano titanium dioxide.
5. An ageing-resistant textile fabric as claimed in claim 2, wherein: the aging resistant agent is prepared by the following steps:
step B1: dissolving cyanuric chloride into ether to prepare cyanuric chloride solution, adding resorcinol and ether into a reaction kettle, stirring at the rotation speed of 120-150r/min and at the temperature of 40-50 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the cyanuric chloride solution, and reacting for 8-10h to prepare an intermediate 1;
step B2: dissolving 2- (2-hydroxy-5-benzyl) benzotriazole in tetrahydrofuran, adding chloroacetyl chloride, reacting for 3-5h at the rotation speed of 200-300r/min and the temperature of 35-40 ℃, adding anhydrous aluminum trichloride and triethylamine, reacting for 3-5h at the rotation speed of 500-800r/min and the temperature of 120-125 ℃ to obtain an intermediate 2, dissolving the intermediate 2 in tetrahydrofuran, adding step B1 to obtain an intermediate 1, and reacting for 2-3h at the temperature of 25-30 ℃ to obtain an intermediate 3;
step B3: adding 3-nitrophenol, 2-nitro-4-hydroxybenzoic acid, anhydrous zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, stirring uniformly at the rotation speed of 120-plus 150r/min, heating to the temperature of 75-80 ℃, reacting for 2-3h, adding deionized water, standing for 20-30min, cooling to the temperature of 15-20 ℃, filtering to remove filtrate to obtain an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, and reacting for 3-5h at the temperature of 85-90 ℃ to obtain an intermediate 5;
step B4: adding the intermediate 5, iron powder and ethanol into a reaction kettle, performing reflux reaction at 80-85 ℃ for 3-5h, adding hydrochloric acid solution for 20min, continuing to react for 5-8h, and adjusting the pH value of the reaction solution to 7-8 to obtain an intermediate 6; adding the intermediate 6 and sulfolane into a reaction kettle, stirring at the rotation speed of 120-plus-150 r/min until the intermediate 6 is completely dissolved, heating to the temperature of 30-35 ℃, introducing phosgene, continuously stirring for 30-50min, heating to the temperature of 120-plus-150 ℃, continuously reacting for 2-3h, cooling to the temperature of 90-100 ℃, introducing nitrogen to remove phosgene, and preserving heat for 10-15min to obtain an intermediate 7;
step B5: dissolving the intermediate 7 in medium tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished to obtain an intermediate 8, dissolving the intermediate 3 in tetrahydrofuran to obtain an intermediate 3 solution, adding resorcinol and diethyl ether into a reaction kettle, stirring at the rotation speed of 120-150r/min and the temperature of 80-90 ℃ until the resorcinol is completely dissolved, adding anhydrous aluminum trichloride and the intermediate 3 solution, reacting for 5-8h, adding the intermediate 8 and the anhydrous potassium manganese carbonate prepared in the step B4, introducing nitrogen for protection, and performing reflux reaction for 5-8h at the temperature of 80-90 ℃ to obtain the anti-aging agent.
6. An ageing-resistant textile fabric as claimed in claim 5, wherein: the molar ratio of the cyanuric chloride to the resorcinol in the step B1 is 1:2, the amount of anhydrous aluminum trichloride is 5-10% of the mass of the cyanuric chloride, the molar ratio of the 2- (2-hydroxy-5-benzyl) benzotriazole, the chloroacetyl chloride and the anhydrous aluminum trichloride in the step B2 is 1:1:1.2, the amount of triethylamine is 3-5% of the mass of the 2- (2-hydroxy-5-benzyl) benzotriazole, the molar ratio of the 3-nitrophenol, the 2-nitro-4-hydroxybenzoic acid, the anhydrous zinc chloride and the phosphorus oxychloride in the step B3 is 1.4:1:1.5:2, the molar ratio of the intermediate 4, the potassium carbonate and the dimethyl sulfate is 3:1:1, the intermediate 5, the iron powder, the ethanol and the hydrochloric acid solution in the step B4 is 2g: 4.5: 60mL:10mL, the volume fraction of ethanol is 90%, the hydrochloric acid solution is concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% are mixed according to the volume ratio of 1:9, the molar ratio of the intermediate 6 to phosgene is 1:1, the molar ratio of the intermediate 7 to boron tribromide in the step B5 is 1g:3mL, the molar ratio of the intermediate 3, resorcinol and the intermediate 8 is 1:1:1, the amount of anhydrous aluminum trichloride is 5-10% of the mass of the intermediate 3, and the amount of anhydrous potassium manganese carbonate is 3-5% of the mass of the intermediate 8.
7. The method for preparing an aging-resistant textile fabric according to claim 1, characterized in that: the polyester fabric is prepared from polyester gray cloth, a first impregnation liquid and a second impregnation liquid, and comprises the following specific steps:
step S1: soaking the terylene gray cloth in a dopamine solution for 20-24h at the temperature of 25-30 ℃;
step S2: padding the treated polyester gray cloth in a first impregnation liquid, and padding for 5-8h at the temperature of 120-150 ℃ to obtain first padded polyester gray cloth;
step S3: padding the first padding terylene grey cloth prepared in the step S2 in a second impregnation liquid, padding for 5-8h at the temperature of 120-150 ℃, and drying at the temperature of 180 ℃ to obtain the anti-aging textile fabric.
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| CN113200942A (en) * | 2021-05-12 | 2021-08-03 | 上绍同烯达(绍兴)新材料科技有限公司 | Antioxidant and method for preparing antioxidant |
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| CN113786287A (en) * | 2021-08-31 | 2021-12-14 | 福建恒安集团有限公司 | Paper diaper and preparation method thereof |
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2020
- 2020-11-05 CN CN202011223240.XA patent/CN112281492A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113200942A (en) * | 2021-05-12 | 2021-08-03 | 上绍同烯达(绍兴)新材料科技有限公司 | Antioxidant and method for preparing antioxidant |
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| CN113308070A (en) * | 2021-07-12 | 2021-08-27 | 安庆市悦发管业有限公司 | Preparation method of anti-ultraviolet PVC drain pipe |
| CN113786287A (en) * | 2021-08-31 | 2021-12-14 | 福建恒安集团有限公司 | Paper diaper and preparation method thereof |
| CN113786287B (en) * | 2021-08-31 | 2022-07-05 | 福建恒安集团有限公司 | Paper diaper and preparation method thereof |
| CN117467125A (en) * | 2023-12-28 | 2024-01-30 | 河南源宏高分子新材料有限公司 | Polyester material for ageing-resistant film and preparation method thereof |
| CN117467125B (en) * | 2023-12-28 | 2024-03-08 | 河南源宏高分子新材料有限公司 | Polyester material for ageing-resistant film and preparation method thereof |
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