CN115450045B - Flame retardant, washable flame-retardant cotton fabric, preparation method and application thereof - Google Patents

Flame retardant, washable flame-retardant cotton fabric, preparation method and application thereof Download PDF

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CN115450045B
CN115450045B CN202210967534.6A CN202210967534A CN115450045B CN 115450045 B CN115450045 B CN 115450045B CN 202210967534 A CN202210967534 A CN 202210967534A CN 115450045 B CN115450045 B CN 115450045B
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cotton fabric
flame retardant
concentration
flame
retardant
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CN115450045A (en
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拜永孝
蔡慧卓
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Lanzhou University
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Lanzhou University
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The application discloses a flame retardant, a washable flame-retardant cotton fabric, a preparation method and application thereof. The flame retardant of the application comprises the following components: graphene oxide, phosphoric acid, urea, guanidine phosphate, dicyandiamide and an aqueous solvent; in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml. The flame retardant is combined with cotton fabric fiber molecules in a multiple bonding mode to form the washable flame-retardant cotton fabric with a three-dimensional penetrating structure. The washable flame-retardant cotton fabric prepared by the method has excellent flame retardant property, LOI (Low-loss-of-ignition) after 50 times of washing can still reach 32.8%, has excellent flame retardant property and washable property, and is simple in preparation process, environment-friendly in preparation process and easy to realize large-scale production.

Description

Flame retardant, washable flame-retardant cotton fabric, preparation method and application thereof
Technical Field
The application belongs to the technical field of functional textiles, and particularly relates to a flame retardant, a washable flame-retardant cotton fabric, a preparation method and application thereof.
Background
In the world, a large number of fire accidents occur each year, bringing serious harm to human life, and a large number of fire accidents are caused by flammable textiles. The cotton fabric has good air permeability, comfort, hydrophilicity, biodegradability and other excellent properties, is widely applied to textile and clothing industries, but has a Limiting Oxygen Index (LOI) of about 18%, and belongs to inflammables. Therefore, the preparation of the cotton fabric with flame retardant property can reduce the fire hazard possibly caused by the cotton fabric in the use process, and is a research subject with practical significance.
The cotton fabric belongs to natural fiber textiles, and the most widely used method is to use a flame retardant to carry out post-treatment on the cotton fabric, namely, the flame retardant is fixed on the surface of the fabric through a layer-by-layer self-assembly method, a chemical grafting method, a sol-gel method and a physical attachment effect, so that the cotton fabric has good flame retardant performance, but the flame retardant cotton fabric finished by the post-treatment generally has the problem of water washing resistance which cannot be ignored. As in patent CN 109183408A, the flame-retardant cotton fabric is prepared by adopting a layer-by-layer self-assembly method with polycation sol and anion solution, and although the prepared flame-retardant cotton fabric has a better flame-retardant effect, the preparation process is simple, green and environment-friendly, the water-washing resistance effect of the flame-retardant cotton fabric prepared by the method is not obvious. As in patent CN110117899a, the surface modification of Attapulgite (ATP) is performed by using KH570, then the cotton fabric is grafted by using KH590, and finally the ATP is grafted to the surface of the cotton fabric by a thio-ene click reaction under ultraviolet light irradiation, so as to prepare a flame-retardant cotton fabric, and the obtained cotton fabric has excellent flame-retardant performance, but the preparation method is complex, and the water-washing resistance of the finally obtained flame-retardant cotton fabric is not clear.
Disclosure of Invention
The application aims to overcome the defects of the prior art, and provides a flame retardant, a washable flame-retardant cotton fabric, a preparation method and application thereof, so as to solve the technical problems of complex preparation process, low flame retardant efficiency and poor washability of the traditional flame-retardant cotton fabric.
In order to achieve the above object, according to a first aspect of the present application, there is provided a flame retardant comprising: graphene oxide, phosphoric acid, urea, guanidine phosphate, dicyandiamide and an aqueous solvent; in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
In a second aspect of the present application, there is provided a method for preparing a flame retardant, comprising the steps of: mixing graphene oxide solution, phosphoric acid, urea, guanidine phosphate and dicyandiamide to prepare a flame retardant;
in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
In a third aspect of the application, there is provided the use of a flame retardant in cotton fabrics.
According to a fourth aspect of the application, there is provided a washable and flame retardant cotton fabric, the surface of which contains a flame retardant, the flame retardant containing the following components: graphene oxide, phosphoric acid, urea, guanidine phosphate, dicyandiamide and an aqueous solvent; in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
In a fifth aspect of the present application, a method for preparing a washable flame retardant cotton fabric is provided, comprising the steps of:
pretreating the surface of cotton fabric;
preparing a flame retardant containing graphene oxide solution, phosphoric acid, urea, guanidine phosphate and dicyandiamide; in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml;
and dipping or coating the flame retardant on the surface of the pretreated cotton fabric, and drying to obtain the washable flame-retardant cotton fabric.
Further, the pretreatment process is as follows: and soaking the cotton fabric in an alkaline solution, washing with water to neutrality, and drying.
Further, the alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
Further, the concentration of the alkaline solution is 0.5-2 mol/L.
Further, the temperature of the drying treatment is 150-170 ℃ and the time is 6-10 min.
Compared with the prior art, the application has the following technical effects:
according to the flame retardant disclosed by the application, the graphene oxide is introduced as a carbon source in the intumescent flame retardant, the graphene oxide can play a barrier and separation role in heat and substance transmission in the combustion process, and the composite acid source and the nitrogen source can play a role in flame retardance in a synergistic manner, so that the flame retardance and the water washing resistance of the cotton fabric are improved.
The preparation method of the flame retardant is simple, low in preparation cost, environment-friendly in preparation process and easy to realize large-scale production.
According to the washable flame-retardant cotton fabric, the surface of the cotton fabric is coated with the flame retardant containing graphene oxide, phosphoric acid, urea, guanidine phosphate and dicyandiamide, covalent grafting (P-O-C and C=N-C grafting) between the flame retardant and cotton fabric fiber molecules is constructed in the high-temperature drying process of the flame retardant, meanwhile, self-assembly effect can be achieved between the graphene oxide and the cotton fiber molecules in the flame retardant system, the washable flame-retardant cotton fabric with a three-dimensional penetrating structure is prepared, and the flame retardance and the washable performance of the cotton fabric are synchronously realized.
The washable flame-retardant cotton fabric has the advantages of simple preparation method, low preparation cost, green and environment-friendly preparation process and easy realization of large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present application, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram showing the bonding mode between a flame retardant and cotton fabric fiber molecules provided by an embodiment of the present application;
fig. 2 is an SEM morphology diagram of the washable flame retardant cotton fabrics prepared in example 3 of the present application before (e) and (f) and after (g) and (h) combustion of the pure cotton fabrics.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
In the present application, the term "and/or" describes an association relationship of an association object, which means that three relationships may exist, for example, a and/or B may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. The character "/" generally indicates that the context-dependent object is an "or" relationship.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
It should be understood that, in various embodiments of the present application, the sequence number of each process described above does not mean that the execution sequence of some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weights of the relevant components mentioned in the description of the embodiments of the present application may refer not only to the specific contents of the components, but also to the proportional relationship between the weights of the components, so long as the contents of the relevant components in the description of the embodiments of the present application are scaled up or down within the scope of the disclosure of the embodiments of the present application. Specifically, the mass described in the specification of the embodiment of the application can be mass units known in the chemical industry field such as mu g, mg, g, kg.
The terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated for distinguishing between objects such as substances from each other. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the application. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature.
In a first aspect, embodiments of the present application provide a flame retardant comprising the following components: graphene oxide, phosphoric acid, urea, guanidine phosphate, dicyandiamide and an aqueous solvent; in the mixed solution of the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
According to the embodiment of the application, the graphene oxide is introduced as a carbon source in the intumescent flame retardant, the graphene oxide can play a role in barrier and separation of heat and substance transmission in the combustion process, and the composite acid source (phosphoric acid, guanidine phosphate) and the nitrogen source (urea and guanidine phosphate) play a role in flame retardance in a synergistic manner, so that the flame retardance and the washability of cotton fabrics are improved.
In a second aspect of the embodiment of the present application, there is provided a method for preparing a flame retardant, including the steps of: mixing graphene oxide solution, phosphoric acid, urea, guanidine phosphate and dicyandiamide to prepare a flame retardant;
in the mixed solution of the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
In a specific embodiment of the present application, the preparation of the flame retardant may employ the following steps: adding Graphene Oxide (GO) solution and phosphoric acid (H) into an aqueous solvent 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared.
Wherein, in the mixed solution, the concentration M1 of graphene oxide is 8-10 mg/ml, the concentration M2 of phosphoric acid is 56-84 mg/ml, the concentration M3 of urea is 34-86 mg/ml, the concentration M4 of guanidine phosphate is 22-65 mg/ml, and the concentration M5 of dicyandiamide is 25-75 mg/ml.
The preparation method of the flame retardant is simple, low in preparation cost, environment-friendly in preparation process and easy to realize large-scale production.
In a third aspect of the embodiments of the present application, an application of the flame retardant in flame-retardant cotton fabrics is provided.
According to a fourth aspect of the embodiment of the application, a washable flame-retardant cotton fabric is provided, the surface of the flame-retardant cotton fabric contains a flame retardant, and the flame retardant contains the following components: graphene oxide, phosphoric acid, urea, guanidine phosphate, dicyandiamide and an aqueous solvent; in the mixed solution of the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml.
According to the washable flame-retardant cotton fabric, the surface of the cotton fabric is coated with the flame retardant containing graphene oxide, phosphoric acid, urea, guanidine phosphate and dicyandiamide, covalent grafting (P-O-C and C=N-C grafting) between the flame retardant and cotton fabric fiber molecules is constructed in a high-temperature drying process, and meanwhile self-assembly effect can be achieved between the graphene oxide and the cotton fiber molecules in the flame retardant system, so that the washable flame-retardant cotton fabric with a three-dimensional penetrating structure is prepared, and the flame retardance and the washable performance of the cotton fabric are synchronously realized.
In a fifth aspect of the embodiments of the present application, a method for preparing a washable and flame retardant cotton fabric is provided, comprising the steps of:
(1) Pretreating the surface of cotton fabric;
(2) Preparing a flame retardant containing graphene oxide, phosphoric acid, urea, guanidine phosphate and dicyandiamide; in the mixed solution of the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml;
(3) And (3) dipping or coating the flame retardant on the surface of the pretreated cotton fabric, and drying to obtain the flame-retardant antibacterial cotton fabric.
In the step (2), the pretreatment process is as follows: and soaking the cotton fabric in an alkaline solution, washing with water to neutrality, and drying. In the embodiment of the application, the alkaline solution is sodium hydroxide solution or potassium hydroxide solution. The concentration of the alkaline solution can be selected to be 0.5-2 mol/L.
In the step (3), the temperature of the drying treatment is 150-170 ℃ and the time is 6-10 min. The water on the surface of the fabric is removed by drying treatment, and the high-temperature drying is carried out to realize P-O-C grafting and C=N-C grafting between the flame retardant and cotton fiber molecules. After drying treatment, the surface of the cotton fabric can be repeatedly coated with the flame retardant for a plurality of times, so that better flame retardant and washing resistant effects are achieved. Specifically, in the coating process, a 250-mesh screen auxiliary scraper coating technology can be used for uniformly coating the novel intumescent flame retardant prepared in the step (1) on the front surface of the cotton fabric subjected to pretreatment in the step (2), and drying treatment is carried out; and then coating the back surface, and repeating the operation to obtain the flame-retardant cotton fabric coated on the two surfaces. The self-assembly effect between GO in the flame retardant and cotton fabric fiber molecules is utilized to realize the coating effect on cotton fibers, and meanwhile, P-O-C grafting and C=N-C grafting between the flame retardant and the cotton fiber molecules are realized in the high-temperature drying process, so that the flame retardant cotton fabric is finally obtained (the combination mode between the flame retardant and the cotton fabric fiber molecules is shown in the attached figure 1).
According to the preparation method of the washable flame-retardant cotton fabric, disclosed by the embodiment of the application, the novel intumescent flame retardant is used for carrying out reactive modification on the hydroxyl functional groups on the surface of the cotton fabric, the flame retardant molecules are combined with cotton fiber molecules on the front and back sides of the cotton fabric in a multiple bonding mode, and meanwhile, the flame retardant penetrates through the inside of the woven structure of the cotton fabric to form the washable flame-retardant cotton fabric with a three-dimensional penetrating structure. The compact three-dimensional penetrating structure plays an excellent role in combustion protection for the cotton fabric substrate; the prepared washable flame-retardant cotton fabric has better washable performance.
The washable flame-retardant cotton fabric provided by the embodiment of the application has the advantages of simple preparation method, low preparation cost, green and environment-friendly preparation process and easiness in realization of large-scale production.
The following examples illustrate one flame retardant, washable flame retardant cotton fabric, methods of making and uses thereof in accordance with embodiments of the present application.
Example 1
The embodiment 1 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant cotton fabric comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 77mg/ml, the concentration of guanidine phosphate is 65mg/ml, the concentration of dicyandiamide is 50mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 2
The embodiment 2 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant cotton fabric comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 86mg/ml, the concentration of guanidine phosphate is 65mg/ml, the concentration of dicyandiamide is 75mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 150 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 3
The embodiment 3 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 34mg/ml, the concentration of guanidine phosphate is 65mg/ml, the concentration of dicyandiamide is 75mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant。
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 4
The embodiment 4 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 51mg/ml, the concentration of guanidine phosphate is 22mg/ml, the concentration of dicyandiamide is 50mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 5
The embodiment 5 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 77mg/ml, the concentration of guanidine phosphate is 65mg/ml, the concentration of dicyandiamide is 25mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 6
The embodiment 6 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 77mg/ml, the concentration of guanidine phosphate is 65mg/ml, the concentration of dicyandiamide is 75mg/ml, and stirring reaction is carried out at room temperature (25 ℃)The flame retardant is obtained after 12 hours.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 150 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 7
The embodiment 7 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 56mg/ml, the concentration of urea is 51mg/ml, the concentration of guanidine phosphate is 43mg/ml, the concentration of dicyandiamide is 50mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
Example 8
The embodiment 8 of the application provides a flame retardant, washable flame retardant cotton fabric and a preparation method thereof, and the flame retardant comprises the following steps:
(1) Pretreatment of cotton fabric, activation of hydroxyl groups on cotton fibers
Preparing a 1mol/L NaOH solution, soaking the cotton fabric in the solution for 24 hours, then washing the cotton fabric with deionized water for many times until the surface of the cotton fabric is nearly neutral, and drying the cotton fabric at 80 ℃ for later use.
(2) Preparation of flame retardant
Adding 15mg/ml Graphene Oxide (GO) solution and phosphoric acid (H) 3 PO 4 ) Urea (Urea), guanidine Phosphate (GP) and catalyst dicyandiamide (dic), a flame retardant mixed solution was prepared. In the mixed solution, the concentration of graphene oxide is 8mg/ml, the concentration of phosphoric acid is 84mg/ml, the concentration of urea is 51mg/ml, the concentration of guanidine phosphate is 43mg/ml, the concentration of dicyandiamide is 50mg/ml, and stirring reaction is carried out at room temperature (25 ℃) for 12 hours to obtain the flame retardant.
(3) Preparation of washable flame-retardant cotton fabric
Uniformly coating the novel intumescent flame retardant prepared in the step (2) on the front surface of the cotton fabric subjected to pretreatment in the step (1) by using a 250-mesh screen auxiliary scraper coating technology, and drying for 5min at the temperature of 170 ℃; and then coating the back surface, and repeating the operation for 6 times to obtain the washable flame-retardant cotton fabric with the three-dimensional penetrating structure.
The washing-resistant flame-retardant cotton fabric prepared in example 3 of the present application was subjected to a burning test, and the SEM morphology of the cotton fabric before (e) (f) and after (g) (h) burning was shown in fig. 2. Through SEM (scanning electron microscope) photo comparison of the flame-retardant cotton fabric before and after combustion, it is obvious that the knitting structure of the flame-retardant cotton fabric after combustion still remains quite complete and compact, the foam-like pellets appearing in the graph (h) further illustrate that the intumescent flame retardant plays a flame retardant role, and the photo comparison of the flame-retardant cotton fabric before and after combustion illustrates that the washable flame-retardant cotton fabric prepared by the embodiment of the application has quite good flame retardant performance.
The flame retardant cotton fabrics prepared in examples 1 to 8 of the present application were tested for limiting oxygen index (LOI:%) and water washing resistance, and the results are shown in the following table. Wherein, each test condition is as follows:
limiting oxygen index test: according to GB/T5454-1997 standard of the textile combustion Performance determination-oxygen index method, the test method is characterized in that a test sample is placed under vertical test conditions, and the minimum oxygen concentration (also called limiting oxygen index) of combustion is just maintained in an oxygen-nitrogen mixed gas flow. The sample holder was placed vertically in the combustion vessel on the sample holder, and the upper end of the sample was ignited in an upward flowing stream of oxygen and nitrogen, and its combustion characteristics were observed, and its after-flame time (not more than 2 min) or destruction length (not more than 40 mm) was compared with a prescribed limit value. The lowest oxygen concentration value, expressed as percent oxygen at the time of sustaining combustion, can be measured by testing a series of samples in different oxygen concentrations.
Washing resistance test: the water wash resistance test was completed using a magnetic stirrer and beaker. 500ml of water was added to a 500ml beaker, and the prepared flame-retardant cotton fabric was cut to 5cm×12cm, and placed in the beaker to be washed with stirring water. The rotating speed of the magnetic stirrer is set to 600r/min, and the 10min is 1 time of water washing.
According to the test results of the table, it can be seen that the LOI of the flame retardant cotton fabrics prepared in examples 1-8 is far higher than that of pure cotton fabrics when not washed, which indicates that the flame retardant cotton fabrics prepared in the examples of the application have very excellent flame retardant property, and the LOI of the flame retardant cotton fabrics prepared in examples 1-8 is greater than 18% of that of pure cotton after being washed with water for 50 times. The LOI of the flame-retardant cotton fabrics prepared in the examples 1, 2, 5 and 6 is respectively 32.8%, 28%, 27.5% and 27.1%, and the LOI is more than 27% (the LOI reaches the standard of flame-retardant textiles, namely, the LOI is more than 26%), which shows that the flame-retardant cotton fabrics prepared in the examples have good washing resistance.
The foregoing examples illustrate only a few embodiments of the application, which are described in detail and are not to be construed as limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.

Claims (4)

1. The preparation method of the washable flame-retardant cotton fabric is characterized by comprising the following steps of:
pretreating the surface of cotton fabric; the pretreatment process comprises the following steps: soaking cotton fabric in alkaline solution, washing with water to neutrality, and drying;
preparing a flame retardant containing graphene oxide solution, phosphoric acid, urea, guanidine phosphate and dicyandiamide; in the flame retardant, the concentration of graphene oxide is 8-10 mg/ml, the concentration of phosphoric acid is 56-84 mg/ml, the concentration of urea is 34-86 mg/ml, the concentration of guanidine phosphate is 22-65 mg/ml, and the concentration of dicyandiamide is 25-75 mg/ml;
dipping or coating the flame retardant on the surface of the pretreated cotton fabric, and drying to obtain the washable flame-retardant cotton fabric; the temperature of the drying treatment is 150-170 ℃ and the time is 5 min.
2. The method for preparing a washable and flame retardant cotton fabric of claim 1, wherein the alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution.
3. The method for preparing the washable flame-retardant cotton fabric according to claim 2, wherein the concentration of the alkaline solution is 0.5-2 mol/L.
4. A washable flame retardant cotton fabric prepared by the method of any one of claims 1-3.
CN202210967534.6A 2022-08-12 2022-08-12 Flame retardant, washable flame-retardant cotton fabric, preparation method and application thereof Active CN115450045B (en)

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CN108611880A (en) * 2018-04-27 2018-10-02 新乡市新科防护科技有限公司 A kind of cotton fabric durable flame-retardant, conduction and grey black dye a step processing method

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