CN110592950B - Method for preparing flame-retardant cotton fabric without solvent - Google Patents
Method for preparing flame-retardant cotton fabric without solvent Download PDFInfo
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- CN110592950B CN110592950B CN201910870314.XA CN201910870314A CN110592950B CN 110592950 B CN110592950 B CN 110592950B CN 201910870314 A CN201910870314 A CN 201910870314A CN 110592950 B CN110592950 B CN 110592950B
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- cotton fabric
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- hyperbranched polyester
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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
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
- C08G83/006—After treatment of hyperbranched macromolecules
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- 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
- D06M15/507—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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- 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
Abstract
The invention discloses a method for preparing a cotton fabric flame-retardant finishing agent without a solvent and application thereof. Mixing the hyperbranched polyester with phosphoric acid for reaction to obtain phosphorus-containing hyperbranched polyester; adding urea into the phosphorus-containing hyperbranched polyester for reaction, precipitating with ethanol, and separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester; dissolving the hyperbranched polyester containing phosphorus and nitrogen in deionized water, and adding dicyandiamide to obtain the flame-retardant finishing agent for the cotton fabric. Soaking a cotton fabric in the flame-retardant finishing agent for the cotton fabric, taking out the cotton fabric, and carrying out two-soaking and two-rolling on the cotton fabric; baking the cotton fabric, cleaning the cotton fabric with clear water, and drying to obtain the flame-retardant cotton fabric. The flame-retardant finishing agent does not need any solvent, and the process is environment-friendly and human-friendly. The formaldehyde is not released in the flame-retardant finishing process of the cotton fabric and the using process of the flame-retardant fabric, and in the flame-retardant finishing process, the flame retardant and the cotton fabric form a plurality of firm covalent bonds, so that the cotton fabric has high-efficiency flame retardance and excellent water washing resistance.
Description
Technical Field
The invention relates to a method for preparing a flame-retardant cotton fabric without a solvent, and belongs to the technical field of flame-retardant finishing of textiles.
Background
The cotton fabric has excellent moisture absorption and air permeability, dyeing property and biocompatibility, and soft hand feeling. The application of cotton textiles has penetrated all aspects of science and technology and life, but while the textiles are widely used, the threat of the textiles to the life and property safety of people is gradually expanding. A large number of researches prove that when a fire disaster happens, the flame-retardant textile is used, the escape guarantee time is longer, 75% of heat is released lower than that of the non-flame-retardant textile, 2/3 (expressed by CO value) of toxic gas released by the non-flame-retardant textile is lower than that of the non-flame-retardant textile, no dense smoke is generated, the fire disaster loss is effectively reduced, and the life safety of people is protected. Therefore, after the textile is subjected to flame retardant finishing, the occurrence rate of fire can be reduced, the threat to life and property is reduced, the flame retardant finishing has commercial significance, and more importantly, the personal safety is ensured. The limit oxygen index of cotton is only 18.0, the cotton is flammable fiber, fire caused by the cotton is a serious potential safety hazard, and the development and application of cotton fabric flame-retardant products are problems to be solved urgently.
Although the formaldehyde content in the traditional flame retardant finishing is high, and the harmful gas after combustion is much. For example, the halogen-containing flame retardant has a good flame retardant effect, but during combustion, the halogen-containing flame retardant material is easy to emit irritant and corrosive hydrogen halide gas, and when some halogen-containing flame retardant systems are cracked and combusted at high temperature, toxic polybrominated compounds are generated, which poses a serious threat to life safety; for example, two most common flame retardants in the market, THPC and Pyrovatex CP, which can form covalent bonds with fibers, have excellent flame retardant and durable properties, but both finishing modes have the problems of formaldehyde residue and subsequent formaldehyde release, so that the non-halogenation and non-formalization of flame retardant materials are increasingly regarded as important.
In the phosphorus-nitrogen synergistic flame retardant, a phosphorus-containing component and a nitrogen-containing component are matched according to a certain proportion, wherein phosphorus and nitrogen play a main flame retardant role. When the flame retardant and the flame retardant are used together, the flame retardant effect of the flame retardant is enhanced. During the combustion process, the phosphorus-containing component generates a phosphoric acid substance in a condensed phase, then a phosphoric acid polymer is generated, and the polymer reacts on the degraded polymer through dehydration and esterification, so that the formation of a carbon layer is promoted; the nitrogen-containing component is decomposed at high temperature to generate non-combustible gas, the non-combustible gas and the protective layer formed by the decomposition of the phosphorus-containing component form a heat insulation layer through foaming, and the heat insulation layer is composed of phosphorus and carbon and is in a foam shape, so that the high polymer is expanded, and the heat conductivity is greatly reduced.
The hyperbranched polyester may have a large number of terminal functional groups such as hydroxyl groups and carboxyl groups, and various functions can be imparted to the hyperbranched polyester by modifying the terminal functional groups. The hyperbranched polyester has a large number of terminal hydroxyl groups and is easy to modify. Through a specific modification means, a novel hyperbranched polyester derivative with terminal groups containing phosphorus and nitrogen groups is formed. The flame retardant is applied to cotton fabrics, so that the cotton fabrics obtain a flame retardant function. The flame retardant efficiency can be greatly improved by improving the proportion of the phosphorus and nitrogen groups in the molecule, and a plurality of end groups can react with the hydroxyl of the cotton fabric to form covalent bonds, so that the cotton fabric has excellent water washing resistance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing cotton fabric flame-retardant finishing agent has the problems of formaldehyde residue and subsequent formaldehyde release in the preparation process.
In order to solve the problems, the invention provides a method for preparing a flame-retardant finishing agent for cotton fabrics without a solvent, which is characterized by mixing hyperbranched polyester and phosphoric acid in proportion, continuously stirring, and carrying out heating reaction to obtain phosphorus-containing hyperbranched polyester; adding urea into the phosphorus-containing hyperbranched polyester, condensing and refluxing, precipitating with ethanol after reaction, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying the mixture in vacuum for later use; dissolving the hyperbranched polyester containing phosphorus and nitrogen in deionized water, and adding dicyandiamide to obtain the flame-retardant finishing agent for the cotton fabric.
Preferably, the molar ratio of the hyperbranched polyester to the phosphoric acid is 1: 16.
Preferably, the reaction temperature of the hyperbranched polyester and the phosphoric acid is 120-140 ℃, and the reaction time is 1-4 h.
Preferably, the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1: 16.
Preferably, the temperature of the condensation reflux is 100 ℃, and the reaction time of the phosphorus-containing hyperbranched polyester and the urea is 0.5-2 h.
Preferably, the mass concentration of the dicyandiamide in the cotton fabric flame-retardant finishing agent is 5%.
The invention also provides the application of the cotton fabric flame-retardant finishing agent prepared by the method, which is characterized in that the cotton fabric is soaked in the cotton fabric flame-retardant finishing agent, then the cotton fabric is taken out, and the cotton fabric is subjected to two-soaking and two-rolling; baking the cotton fabric, cleaning the cotton fabric with clear water, and drying to obtain the flame-retardant cotton fabric.
Preferably, the bath ratio of the cotton fabric to the flame-retardant finishing agent for the cotton fabric is 1:20, the dipping temperature is 70 ℃, and the dipping time is 10-30 min.
Preferably, the liquid carrying rate of the cotton fabric after the two-dipping and the two-rolling is 120%.
Preferably, the baking temperature is 170 ℃ and the baking time is 3 min.
The main reaction process for preparing the cotton fabric flame-retardant finishing agent is shown as the following formula:
the main reaction process for preparing the flame-retardant cotton fabric is shown as the following formula:
the flame-retardant finishing agent does not need any solvent, and the process is environment-friendly and human-friendly. The formaldehyde is not released in the flame-retardant finishing process of the cotton fabric and the using process of the flame-retardant fabric, and in the flame-retardant finishing process, the flame retardant and the cotton fabric form a plurality of firm covalent bonds, so that the cotton fabric has high-efficiency flame retardance and excellent water washing resistance.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Example 1
A method for preparing a cotton fabric flame-retardant finishing agent without a solvent comprises the following specific steps:
(1) mixing the hyperbranched polyester and phosphoric acid according to the molar ratio of 1:16, continuously stirring, and reacting for 3h at 120 ℃ to obtain phosphorus-containing hyperbranched polyester;
(2) adding urea into the phosphorus-containing hyperbranched polyester, wherein the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1:16, carrying out condensation reflux at 100 ℃, reacting for 1h, precipitating with ethanol, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying in a vacuum oven at 80 ℃ for later use;
(3) dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, adding dicyandiamide with the mass of 5 wt% of the solution, soaking a cotton fabric in the solution at a bath ratio of 1:20 for 30min at 70 ℃, taking out the cotton fabric, and soaking and rolling the cotton fabric twice to ensure that the liquid carrying rate of the cotton fabric is 120%; and finally, treating the cotton fabric for 3min at 170 ℃ by using an automatic continuous dryer, cleaning the cotton fabric by using clear water, and drying the cotton fabric to obtain the flame-retardant cotton fabric. The cotton fabric can reach the fabric class 1 standard of GB 20286-2006 flame-retardant products and assemblies in public places, requirements and marks.
Example 2
A method for preparing a cotton fabric flame-retardant finishing agent without a solvent comprises the following specific steps:
(1) mixing the hyperbranched polyester and phosphoric acid according to the molar ratio of 1:16, continuously stirring, and reacting for 3h at the temperature of 130 ℃ to obtain phosphorus-containing hyperbranched polyester;
(2) adding urea into the phosphorus-containing hyperbranched polyester, wherein the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1:16, carrying out condensation reflux at 100 ℃, reacting for 1h, precipitating with ethanol, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying in a vacuum oven at 80 ℃ for later use;
(3) dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, adding dicyandiamide with the mass of 5 wt% of the solution, soaking a cotton fabric in the solution at a bath ratio of 1:20 for 30min at 70 ℃, taking out the cotton fabric, and soaking and rolling the cotton fabric twice to ensure that the liquid carrying rate of the cotton fabric is 120%; and finally, treating the cotton fabric for 3min at 170 ℃ by using an automatic continuous dryer, cleaning the cotton fabric by using clear water, and drying the cotton fabric to obtain the flame-retardant cotton fabric.
After 80g/L of flame retardant is used for finishing cotton fabric, the weight of the fabric is increased by 15.5%, the afterflame time and the smoldering time in a vertical combustion test are 0, the length of the damaged carbon is 72mm, the fabric class 1 standard of GB 20286 plus 2006 flame-retardant product and component combustion performance requirement and identification in public places can be reached, after 30 times of water washing, the afterflame and the smoldering do not occur, the length of the damaged carbon is 105mm, and the fabric class 1 standard can still be reached. The combustion and water washing test effect of the finished cotton fabric under the conditions of low concentration and low weight gain shows that the finished cotton fabric has high-efficiency durability.
Example 3
A method for preparing a cotton fabric flame-retardant finishing agent without a solvent comprises the following specific steps:
(1) mixing the hyperbranched polyester and phosphoric acid according to the molar ratio of 1:16, continuously stirring, and reacting for 3h at the temperature of 140 ℃ to obtain phosphorus-containing hyperbranched polyester;
(2) adding urea into the phosphorus-containing hyperbranched polyester, wherein the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1:16, carrying out condensation reflux at 100 ℃, reacting for 1h, precipitating with ethanol, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying in a vacuum oven at 80 ℃ for later use;
(3) dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, adding dicyandiamide with the mass of 5 wt% of the solution, soaking a cotton fabric in the solution at a bath ratio of 1:20 for 30min at 70 ℃, taking out the cotton fabric, and soaking and rolling the cotton fabric twice to ensure that the liquid carrying rate of the cotton fabric is 120%; and finally, treating the cotton fabric for 3min at 170 ℃ by using an automatic continuous dryer, cleaning the cotton fabric by using clear water, and drying the cotton fabric to obtain the flame-retardant cotton fabric.
After the 80g/L flame retardant is used for finishing the cotton fabric, the weight of the fabric is increased by 15.5%, the afterflame time and the smoldering time in a vertical combustion test are 0, the length of the damaged carbon is 72mm, the fabric class 1 standard of GB 20286 plus 2006 flame-retardant product and component combustion performance requirement and identification in public places can be reached, after 30 times of water washing, the afterflame and the smoldering do not occur, the length of the damaged carbon is 105mm, the class 1 standard can still be reached, and the durability of the finished cotton fabric is good.
Example 4
A method for preparing a cotton fabric flame-retardant finishing agent without a solvent comprises the following specific steps:
(1) mixing the hyperbranched polyester and phosphoric acid according to the molar ratio of 1:16, continuously stirring, and reacting for 3h at the temperature of 130 ℃ to obtain phosphorus-containing hyperbranched polyester;
(2) adding urea into the phosphorus-containing hyperbranched polyester, wherein the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1:16, carrying out condensation reflux at 100 ℃, reacting for 2 hours, precipitating with ethanol, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying in a vacuum oven at 80 ℃ for later use;
(3) dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, adding dicyandiamide with the mass of 5 wt% of the solution, soaking a cotton fabric in the solution at a bath ratio of 1:20 for 30min at 70 ℃, taking out the cotton fabric, and soaking and rolling the cotton fabric twice to ensure that the liquid carrying rate of the cotton fabric is 100%; and finally, treating the cotton fabric for 3min at 170 ℃ by using an automatic continuous dryer, cleaning the cotton fabric by using clear water, and drying the cotton fabric to obtain the flame-retardant cotton fabric.
After the 120g/L flame retardant finishes the cotton fabric, the after-burning time and smoldering time in a vertical burning test are 0, the length of the damaged carbon is 62mm, the fabric class 1 standard of GB 20286 plus 2006 flame-retardant product and component burning performance requirement and identification in public places can be reached, after 30 times of water washing, the after-burning and smoldering do not occur, the length of the damaged carbon is 80mm, the grade 1 standard can still be reached, and the durability of the finished cotton fabric is good.
Example 5
A method for preparing a cotton fabric flame-retardant finishing agent without a solvent comprises the following specific steps:
(1) mixing the hyperbranched polyester and phosphoric acid according to the molar ratio of 1:16, continuously stirring, and reacting for 1h at the temperature of 130 ℃ to obtain phosphorus-containing hyperbranched polyester;
(2) adding urea into the phosphorus-containing hyperbranched polyester, wherein the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1:16, carrying out condensation reflux at 100 ℃, reacting for 1h, precipitating with ethanol, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying in a vacuum oven at 80 ℃ for later use;
(3) dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, adding dicyandiamide with the mass of 5 wt% of the solution, soaking a cotton fabric in the solution at a bath ratio of 1:20 for 30min at 70 ℃, taking out the cotton fabric, and soaking and rolling the cotton fabric twice to ensure that the liquid carrying rate of the cotton fabric is 120%; and finally, treating the cotton fabric for 3min at 170 ℃ by using an automatic continuous dryer, cleaning the cotton fabric by using clear water, and drying the cotton fabric to obtain the flame-retardant cotton fabric.
After 200g/L of flame retardant finishes cotton fabric, the afterflame time and smoldering time in a vertical combustion test are 0, the length of the damaged carbon is 48mm, the fabric class 1 standard of GB 20286 plus 2006 flame retardant product and component combustion performance requirement and identification in public places can be reached, after 30 times of water washing, afterflame and smoldering do not occur, the length of the damaged carbon is 68mm, the class 1 standard can still be reached, and the durability of the finished cotton fabric is good.
Claims (6)
1. A method for preparing a flame-retardant finishing agent for cotton fabrics without a solvent is characterized in that hyperbranched polyester and phosphoric acid are mixed according to a proportion, continuously stirred and heated for reaction to obtain phosphorus-containing hyperbranched polyester; adding urea into the phosphorus-containing hyperbranched polyester, condensing and refluxing, precipitating with ethanol after reaction, separating and purifying the phosphorus-containing hyperbranched polyester and the nitrogen-containing hyperbranched polyester, and drying the mixture in vacuum for later use; dissolving hyperbranched polyester containing phosphorus and nitrogen in deionized water, and adding dicyandiamide to obtain a cotton fabric flame-retardant finishing agent; the molar ratio of the hyperbranched polyester to the phosphoric acid is 1: 16; the reaction temperature of the hyperbranched polyester and the phosphoric acid is 120-140 ℃, and the reaction time is 1-4 h; the molar ratio of the phosphorus-containing hyperbranched polyester to the urea is 1: 16; the temperature of the condensation reflux is 100 ℃, and the reaction time of the phosphorus-containing hyperbranched polyester and the urea is 0.5-2 h.
2. The method for preparing the cotton fabric flame-retardant finishing agent without the solvent according to claim 1, wherein the mass concentration of the dicyandiamide in the cotton fabric flame-retardant finishing agent is 5%.
3. The use of a cotton fabric flame retardant finish prepared by the method of any one of claims 1-2, characterized in that a cotton fabric is dipped in the cotton fabric flame retardant finish, then the cotton fabric is taken out and subjected to two dipping and two rolling; baking the cotton fabric, cleaning the cotton fabric with clear water, and drying to obtain the flame-retardant cotton fabric.
4. The use of claim 3, wherein the cotton fabric is impregnated in the flame retardant finishing agent for the cotton fabric at a bath ratio of 1:20, at a temperature of 70 ℃ for a time of 10-30 min.
5. The use of claim 3, wherein the liquor pick-up of said cotton fabric after double soaking and double rolling is 120%.
6. The use according to claim 3, wherein the baking temperature is 170 ℃ and the baking time is 3 min.
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| CN115679689A (en) * | 2022-12-12 | 2023-02-03 | 杨开健 | Flame-retardant fabric finishing agent and fabric finishing method |
| CN116397438B (en) * | 2023-03-14 | 2024-03-15 | 苏州大学 | Durable flame-retardant polyester/cotton blended fabric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012022407A1 (en) * | 2010-08-18 | 2012-02-23 | Merck Patent Gmbh | Composition containing hyperbranched polymers |
| CN106633022A (en) * | 2016-11-28 | 2017-05-10 | 宋雪晶 | Preparation method and application of three-source integrated hyperbranched structure flame retardant |
| CN110016130A (en) * | 2019-04-01 | 2019-07-16 | 东华大学 | The preparation method of phosphorus, nitrogen type flame retardant and flame-retardant textile based on hyper-branched polyester |
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| US20170073465A1 (en) * | 2014-02-28 | 2017-03-16 | Michigan Molecular Institute | Sustained release composition using biobased biodegradable hyperbranched polyesters |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012022407A1 (en) * | 2010-08-18 | 2012-02-23 | Merck Patent Gmbh | Composition containing hyperbranched polymers |
| CN106633022A (en) * | 2016-11-28 | 2017-05-10 | 宋雪晶 | Preparation method and application of three-source integrated hyperbranched structure flame retardant |
| CN110016130A (en) * | 2019-04-01 | 2019-07-16 | 东华大学 | The preparation method of phosphorus, nitrogen type flame retardant and flame-retardant textile based on hyper-branched polyester |
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