CN116284640A - Preparation method of flame-retardant waterborne polyurethane finishing agent for polyester fabric - Google Patents

Preparation method of flame-retardant waterborne polyurethane finishing agent for polyester fabric Download PDF

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CN116284640A
CN116284640A CN202211575919.4A CN202211575919A CN116284640A CN 116284640 A CN116284640 A CN 116284640A CN 202211575919 A CN202211575919 A CN 202211575919A CN 116284640 A CN116284640 A CN 116284640A
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flame
waterborne polyurethane
polyester
retardant waterborne
retardant
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沈青青
万军民
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Zhejiang Sci Tech University ZSTU
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Zhejiang Sci Tech University ZSTU
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3271—Hydroxyamines
    • C08G18/3278—Hydroxyamines containing at least three hydroxy groups
    • C08G18/3281—Hydroxyamines containing at least three hydroxy groups containing three hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348—Hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
    • C08G18/3878—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/83—Chemically modified polymers
    • C08G18/831—Chemically modified polymers by oxygen-containing compounds inclusive of carbonic acid halogenides, carboxylic acid halogenides and epoxy halides
    • 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
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
    • D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M14/32—Polyesters
    • 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
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • 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
    • 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
    • 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
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Abstract

The invention relates to the technical field of flame-retardant waterborne polyurethane finishing agents, and discloses a preparation method of a flame-retardant waterborne polyurethane finishing agent for polyester fabrics, which comprises the following steps: mixing Exolit OP 550, polyethylene glycol 300, isophorone diisocyanate and a catalyst, heating in water bath, stirring, setting the temperature to 80-90 ℃, and reacting for 1-3h; adding dimethylolpropionic acid and pentaerythritol for chain extension, adding triethanolamine for reaction, and then dropwise adding an ethanol water solution containing sodium bisulphite for end capping to obtain flame-retardant waterborne polyurethane; irradiating the polyester fabric subjected to alkali treatment with ultraviolet light under the initiation of a photoinitiator, and then adding N-methylolacrylamide for photo-grafting to obtain modified polyester; and then performing flame-retardant finishing on the modified polyester by using the obtained flame-retardant waterborne polyurethane. The polyester fabric subjected to flame retardant finishing can be effectively flame retardant and molten drop resistant, and the flame retardant performance of the polyester fabric is not weakened due to water washing.

Description

Preparation method of flame-retardant waterborne polyurethane finishing agent for polyester fabric
Technical Field
The invention belongs to the technical field of flame-retardant waterborne polyurethane finishing agents, and particularly relates to a preparation method of a flame-retardant waterborne polyurethane finishing agent for polyester fabrics.
Background
The polyester fiber has high strength, high modulus and low water absorption, and has wide application as civil fabric and industrial fabric. However, terylene is easy to ignite, black smoke is emitted while melting during combustion, curling occurs, and the terylene is melted into beads, so that great potential safety hazards are caused in the application process.
Polyurethane is an organic high molecular polymer containing carbamate chain segment structural units, which is prepared by reacting isocyanate with polyester or polyether polyol. The aqueous polyurethane is a polyurethane system which uses water instead of an organic solvent as a dispersion medium. The aqueous polyurethane resin is a uniform emulsion formed by dispersing polyurethane in water, has the advantages of incombustibility, small smell, no pollution to environment, energy conservation, convenient operation and processing and the like, and is widely used as an adhesive and a coating. Therefore, the polyurethane can be used as an effective flame-retardant polyester fabric finishing agent.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a flame-retardant waterborne polyurethane finishing agent for polyester fabrics, which is used for finishing waterborne flame-retardant polyurethane on the polyester fabrics, can effectively resist flame and molten drops, and ensures that the flame retardant performance of the flame-retardant waterborne polyurethane finishing agent is not weakened due to water washing.
In order to achieve the above purpose, the invention provides a preparation method of a flame-retardant waterborne polyurethane finishing agent for polyester fabrics, which comprises the following steps:
step one: mixing Exolit OP 550, polyethylene glycol 300, isophorone diisocyanate and a catalyst, heating in water bath, stirring, setting the temperature to 80-90 ℃, and reacting for 1-3h;
step two: the set temperature is reduced to 70-80 ℃, dimethylolpropionic acid and pentaerythritol are added, and after the viscosity is regulated by a solvent, the reaction is carried out for 1-3 hours;
step three: reducing the set temperature to 50-60 ℃, adding triethanolamine, and reacting for 0.5-1h;
step four: placing the reactant in the third step in an ice water bath at 0-5 ℃, adding a solvent, then dropwise adding an ethanol water solution containing sodium bisulphite, and reacting for 2-3 hours to obtain flame-retardant waterborne polyurethane;
step five: after alkali treatment is carried out on the polyester fabric, taking out, washing and drying;
step six: under the irradiation of ultraviolet light and the initiation of a photoinitiator, N-methylol acrylamide is introduced to carry out light grafting on the polyester fabric subjected to alkali treatment, so as to obtain modified polyester;
step seven: diluting the flame-retardant waterborne polyurethane obtained in the step four with water, adding modified polyester, oscillating for 20-30min in a water bath at 40-50 ℃, pre-drying for 5-8min at 70-75 ℃, and then baking for 3-8min at 140-145 ℃.
The invention firstly makes Exolit OP 550, polyethylene glycol and isophorone diisocyanate react with polyester at high temperature, then adds dimethylolpropionic acid and pentaerythritol for chain extension, and then uses sodium bisulphite for end capping of aqueous polyurethane to prepare flame-retardant aqueous polyurethane. The durability of the polyurethane chain extension by adopting the dimethylolpropionic acid and the pentaerythritol is better, and the bonding property of the polyurethane chain extension with modified polyester is better because the crosslinking degree after chain extension is larger and the proportion of grafting end capping is higher. And the sodium bisulphite is used for blocking, the blocked polyurethane can be better combined with polyester fabrics, the combination stability is improved, and the flame retardant effect of the polyester after washing is prevented from disappearing. Then, when the flame-retardant waterborne polyurethane is used for polyester fabrics, ultraviolet irradiation is carried out on the surfaces of the polyester fabrics, and N-methylol acrylamide is grafted, so that the polyester fabrics can resist molten drops in the process of burning, and introduced hydroxyl can react with the waterborne polyurethane in the process of post-treatment, and the flame-retardant performance of the flame-retardant waterborne polyurethane is not weakened due to water washing while flame retardance is ensured.
The prepared flame-retardant waterborne polyurethane emulsion has high solid content and good water solubility, and the waterborne flame-retardant polyurethane can be effectively flame-retardant, anti-dripping, and can be extinguished when the cloth is separated from fire, and has no black smoke during combustion, thereby being environment-friendly. The flame-retardant finished polyester fabric is subjected to a vertical burning test according to a GB 5455-1997 method, the continuous burning time is 0 second, the smoldering time is 0 second, the damage length is 44mm-46mm, the limiting oxygen index is 27-29%, and the flame-retardant effect after 50 times of water washing is still obvious.
Further preferably, in step oneThe content of phosphorus in the Exolit OP 550 is 16-18%, and the density at 25 ℃ is 1.3g/cm 3 The hydroxyl number was 170mg KOH/g.
Further preferably, in the first step, the mass ratio of Exolit OP 550, isophorone diisocyanate, and polyethylene glycol 300 is 1:1:0.5; the catalyst is dibutyl tin dilaurate.
Further preferably, in the second step, the adding amount of the dimethylolpropionic acid is 10-11% of the total mass of the raw materials in the first step; the addition amount of the pentaerythritol is 7-8% of the total mass of the raw materials in the first step.
In addition, in the second step, medicines cannot be added immediately when the temperature of the water bath is adjusted to 70-80 ℃, and medicines can be added when the temperature of the system is reduced to 70-80 ℃ and a small amount of solvent is used for adjusting the viscosity of the system to prevent the system from solidifying.
Further preferably, in step three, the amount of the triethanolamine to dimethylolpropionic acid material is 1:1.
And step three, adding triethanolamine to replace carboxyl of the dimethylolpropionic acid, neutralizing the dimethylolpropionic acid added in the step three, and increasing the hydrophilicity of the polyurethane.
Further preferably, in step four, the ratio of the sodium bisulphite to the amount of the substance of isophorone diisocyanate is 1:1.
Further preferably, in the fifth step, the alkali treatment of the polyester fabric is as follows: placing the polyester fabric into finishing liquid containing 40-45g/L NaOH and 0.5-1g/L cetyltrimethylammonium bromide, and soaking in 80-85deg.C water bath for 50-60min.
Further preferably, in the step six, the addition amount of the photoinitiator is 2-10% of the mass of the polyester fabric. The total mass of the polyester fabric is optimized to be 2-5%, and the total mass of the polyester fabric is further optimized to be 3%.
Further preferably, in the sixth step, the illumination time of the ultraviolet light is 3-10min.
Further preferably, in the seventh step, the mass ratio of the flame retardant waterborne polyurethane to water is 1:2-3 when the flame retardant waterborne polyurethane is diluted by water.
Compared with the prior art, the invention has the following advantages: the water-based flame-retardant polyurethane is arranged on the modified polyester fabric, can effectively resist flame and molten drops, is extinguished immediately after the cloth is separated from fire, is free from black smoke during combustion, is environment-friendly, and ensures that the flame retardant performance of the water-based flame-retardant polyurethane is not weakened due to water washing while being flame-retardant.
Detailed Description
The technical contents and effects of the present invention will be further described in detail with reference to examples, but the present invention is not limited thereto.
Example 1
Step one: 40g of Exolit OP 550, 20g of polyethylene glycol 300 and 41g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; pentaerythritol 7.4g and dimethylolpropionic acid 10.5g were weighed out and 10.5g dimethylolpropionic acid was dissolved using 15mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 75 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 11.6g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 18.7g of sodium bisulphite is weighed and dissolved in 290mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the obtained solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃.
Example 2
Step one: 50g of Exolit OP 550, 25g of polyethylene glycol 300 and 50g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; pentaerythritol 9.1g and dimethylolpropionic acid 13.8g were weighed out and 13.8g dimethylolpropionic acid was dissolved using 20mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 75 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 15.3g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 22.9g of sodium bisulphite is weighed and dissolved in 300mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel in a dropwise manner, and the reaction is carried out for 2.5h, thus obtaining the flame-retardant waterborne polyurethane.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: : weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the obtained solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃.
Example 3
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 11.0g of pentaerythritol and 16.5g of dimethylolpropionic acid were weighed out, and 16.5g of dimethylolpropionic acid was dissolved using 25mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 75 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 18.4g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 28.1g of sodium bisulphite is weighed and dissolved in 330mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: : weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃.
Control example 1 (untreated polyester fabrics)
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 11.0g of pentaerythritol and 16.5g of dimethylolpropionic acid were weighed out, and 16.5g of dimethylolpropionic acid was dissolved using 25mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 70 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 18.4g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 28.1g of sodium bisulphite is weighed and dissolved in 330mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step five: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking strip-shaped dry and clean polyester cloth with the width of 30mm and the mass of 30g in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using an oven, and baking for 4min at 140 ℃.
Control 2 (polyurethane not blocked with sodium bisulfite)
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 11.0g of pentaerythritol and 16.5g of dimethylolpropionic acid were weighed out, and 16.5g of dimethylolpropionic acid was dissolved using 25mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 70 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 18.4g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: and (3) placing the three-neck flask into an ice-water bath, cooling the system to 3 ℃, then adding the system into 330mL of deionized water, and emulsifying for 30min to obtain the flame-retardant waterborne polyurethane.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: : weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the obtained solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃. Control example 3 (too little sodium bisulfite for polyurethane termination)
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 11.0g of pentaerythritol and 16.5g of dimethylolpropionic acid were weighed out, and 16.5g of dimethylolpropionic acid was dissolved using 25mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 70 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 18.4g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 14.05g of sodium bisulphite is weighed and dissolved in 330mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the obtained solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 Irradiating with ultraviolet light, and photo-grafting polyester with N-methylolacrylamide to obtain modified polyesterPolyester.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃. Comparative example 4 (polyurethane chain extension with butanediol)
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 27.5g of butanediol was weighed out and 16.5g of dimethylolpropionic acid was dissolved using 35mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 70 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the stirrer is not turned off, the temperature of the constant-temperature water bath kettle is adjusted to 55 ℃, 18.4g of triethanolamine is weighed, and when the temperature of the system in the three-neck flask is reduced to 55 ℃, the triethanolamine is added into the three-neck flask, and the reaction is carried out for 0.5h.
Step four: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 28.1g of sodium bisulphite is weighed and dissolved in 330mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step five: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step six: weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step seven: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step four, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃.
Comparative example 5 (preparation of polyurethane without triethanolamine)
Step one: 60g of Exolit OP 550, 30g of polyethylene glycol 300 and 60g of isophorone diisocyanate are weighed and put into a three-neck flask with a stirrer, the three-neck flask is fixed in a constant-temperature water bath kettle, the temperature is set at 85 ℃, 0.05g of dibutyltin dilaurate catalyst with the purity of 95% is added, and stirring is started to fully mix materials for 2 hours.
Step two: the stirrer is not closed, the temperature of the constant-temperature water bath kettle is adjusted to 75 ℃, and the system in the three-neck flask is waited for cooling; 11.0g of pentaerythritol and 16.5g of dimethylolpropionic acid were weighed out, and 16.5g of dimethylolpropionic acid was dissolved using 25mL of N-methylpyrrolidone (NMP) which was used to adjust the viscosity of the system; when the temperature of the system in the three-neck flask is reduced to 70 ℃, adding the weighed medicines into the three-neck flask, and continuing to react for 2 hours.
Step three: the three-necked flask was placed in an ice-water bath, the temperature of the system was lowered to 3℃and 10mL of ethyl acetate was added. 28.1g of sodium bisulphite is weighed and dissolved in 330mL of deionized water, 33mL of ethanol is added for uniform mixing, then the ethanol water solution containing sodium bisulphite is added into a three-neck flask by a constant pressure dropping funnel for reaction for 2.5h, and the flame-retardant waterborne polyurethane is obtained.
Step four: alkali treatment is carried out on the polyester fabric, 1000g of dry clean polyester fabric is taken, polyester is arranged in finishing liquid with the mass concentration of NaOH of 40g/L and the mass concentration of hexadecyl trimethyl ammonium bromide active agent of 1g/L, water bath heating at 80 ℃ is adopted, the polyester fabric is immersed in the finishing liquid for 50min, and the polyester fabric is taken out, washed and dried.
Step five: weighing 30g of photo initiator TPO and 30g of N-methylolacrylamide, dissolving with 1000mL of deionized water, soaking 1000g of polyester cloth subjected to alkali treatment in the solution, and under the initiation of the photo initiator TPO, adopting a MUA-165 ultraviolet irradiation device, wherein the UV irradiance is 3800mW/cm 2 The N-methylolacrylamide is irradiated by ultraviolet light, and the dacron is subjected to light grafting to obtain the modified dacron.
Step six: measuring 30mL of the flame-retardant waterborne polyurethane obtained in the step three, and then adding 60mL of deionized water to complete the configuration of the working solution; soaking 30mm wide and 30g long modified polyester in a working solution, oscillating for 30min in a water bath at 40 ℃, pre-baking for 5min at 70 ℃ by using a baking oven, and baking for 4min at 140 ℃.
TABLE 1
Figure BDA0003988150170000091
Figure BDA0003988150170000101
In Table 1, the flame retardant effect is a vertical burning test of the fabric according to the standard GB 5455-1997; the flame retardant effect after 50 times of water washing is compared with the flame retardant effect before water washing, and the water bath ratio of each time is 1:20.
as can be seen from Table 1, the modified polyester fabric is grafted with N-methylolacrylamide to effectively resist molten drops, and the hydroxyl groups on the modified polyester can be combined with the end-capped flame-retardant waterborne polyurethane in a reaction manner more firmly, so that the water-washing resistance is improved, and the flame-retardant waterborne polyurethane still has flame retardant property after 50 times of water washing. As is clear from comparison of example 1 and comparative example 2, the polyurethane without the end cap has flame retardant effect, but it cannot react with hydroxyl groups on the modified polyester, so that the flame retardant effect of the modified polyester disappears after washing with water. As is clear from the comparison of example 1 with comparative example 3, the amount of the end-capping agent added was reduced, and the polyurethane was not totally end-capped, so that the amount of polyurethane reacted with the modified polyester was also reduced, and the flame retarding effect was poor after 50 water washes. As is clear from the comparison of example 1 with comparative example 4, the polyurethane chain-extended with dimethylolpropionic acid and pentaerythritol has better durability because the degree of crosslinking after chain extension is greater and the proportion of graft end capping is higher, so that it has better bonding with the modified polyester. And after the chain is extended by 1,4 butanediol, the durability of the polyurethane is poor, and the flame retardant effect is poor after 50 times of water washing. As is clear from the comparison between the examples and the comparative example 5, the triethanolamine mainly serves to neutralize the added dimethylolpropionic acid and increase the hydrophilicity of the polyurethane during the preparation of the polyurethane, and the polyurethane obtained in the comparative example 5 has poor hydrophilicity without adding triethanolamine during the preparation of the polyurethane. In the finishing process of the modified polyester, the water solubility is poor, the combination effect is poor, so that the flame retardant effect is obviously reduced, and the flame retardant effect disappears after water washing.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. Not all embodiments are exhaustive. Obvious changes and modifications which are extended by the technical proposal of the invention are still within the protection scope of the invention.

Claims (10)

1. The preparation method of the flame-retardant waterborne polyurethane finishing agent for the polyester fabric is characterized by comprising the following steps of:
step one: mixing Exolit OP 550, polyethylene glycol 300, isophorone diisocyanate and a catalyst, heating in water bath, stirring, setting the temperature to 80-90 ℃, and reacting for 1-3h;
step two: the set temperature is reduced to 70-80 ℃, dimethylolpropionic acid and pentaerythritol are added, and after the viscosity is regulated by a solvent, the reaction is carried out for 1-3 hours;
step three: reducing the set temperature to 50-60 ℃, adding triethanolamine, and reacting for 0.5-1h;
step four: placing the reactant in the third step in an ice water bath at 0-5 ℃, adding a solvent, then dropwise adding an ethanol water solution containing sodium bisulphite, and reacting for 2-3 hours to obtain flame-retardant waterborne polyurethane;
step five: after alkali treatment is carried out on the polyester fabric, taking out, washing and drying;
step six: under the irradiation of ultraviolet light and the initiation of a photoinitiator, N-methylol acrylamide is introduced to carry out light grafting on the polyester fabric subjected to alkali treatment, so as to obtain modified polyester;
step seven: diluting the flame-retardant waterborne polyurethane obtained in the step four with water, adding modified polyester, oscillating for 20-30min in a water bath at 40-50 ℃, pre-drying for 5-8min at 70-75 ℃, and then baking for 3-8min at 140-145 ℃.
2. The method for preparing flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the first step, the phosphorus content in the Exolit OP 550 is 16-18%, and the density at 25 ℃ is 1.3g/cm 3 The hydroxyl number was 170mg KOH/g.
3. The method for preparing the flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1 or 2, wherein in the first step, the mass ratio of Exolit OP 550, isophorone diisocyanate and polyethylene glycol 300 is 1:1:0.5; the catalyst is dibutyl tin dilaurate.
4. The method for preparing the flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the second step, the adding amount of the dimethylolpropionic acid is 10-11% of the total mass of the raw materials in the first step; the addition amount of the pentaerythritol is 7-8% of the total mass of the raw materials in the first step.
5. The method for preparing a flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the third step, the ratio of the amount of triethanolamine to the amount of dimethylolpropionic acid is 1:1.
6. The method for preparing a flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the fourth step, the ratio of the amount of sodium bisulphite to the amount of the substance of isophorone diisocyanate is 1:1.
7. the method for preparing the flame retardant waterborne polyurethane finishing agent for the polyester fabric according to claim 1, wherein in the fifth step, the polyester fabric is subjected to alkali treatment as follows: placing the polyester fabric into finishing liquid containing 40-45g/L NaOH and 0.5-1g/L cetyltrimethylammonium bromide, and soaking in 80-85deg.C water bath for 50-60min.
8. The method for preparing a flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the sixth step, the addition amount of the photoinitiator is 2-10% of the mass of the polyester fabrics.
9. The method for preparing a flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1 or 8, wherein in the sixth step, the irradiation time of ultraviolet light is 3-10min.
10. The method for preparing a flame retardant waterborne polyurethane finishing agent for polyester fabrics according to claim 1, wherein in the seventh step, when the flame retardant waterborne polyurethane is diluted with water, the mass ratio of the flame retardant waterborne polyurethane to the water is 1:2-3.
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