CN118668472B - Graphite-based flame retardant, graphite-based flame retardant finishing liquid, and preparation method and application thereof - Google Patents
Graphite-based flame retardant, graphite-based flame retardant finishing liquid, and preparation method and application thereof Download PDFInfo
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- CN118668472B CN118668472B CN202411156312.1A CN202411156312A CN118668472B CN 118668472 B CN118668472 B CN 118668472B CN 202411156312 A CN202411156312 A CN 202411156312A CN 118668472 B CN118668472 B CN 118668472B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/61—Polyamines polyimines
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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
- 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
- D06M2101/34—Polyamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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Abstract
The invention belongs to the technical field of flame retardance, and in particular relates to a graphite-based flame retardant, a graphite-based flame retardant finishing liquid and a preparation method and application thereof, wherein the preparation method of the graphite-based flame retardant finishing liquid comprises the steps of firstly preparing a reaction system a which simultaneously contains expandable graphite, dopamine hydrochloride, hydrogen peroxide and a solvent and has a pH value of more than 7, and then reacting for 1-2 hours at 70-80 ℃; and adding glucose into the reaction system a to obtain a reaction system b, reacting at 80-90 ℃ to obtain a graphite-based flame retardant finishing liquid, purifying the graphite-based flame retardant finishing liquid to obtain a graphite-based flame retardant, and reacting the graphite-based flame retardant finishing liquid with nylon 6 fabric at 80-90 ℃ to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric. The halogen-free phosphorus-free flame-retardant nylon 6 fabric prepared by the method has good flame-retardant effect, and has good flame-retardant effect after 20 times of water washing.
Description
Technical Field
The invention belongs to the technical field of flame retardance, and particularly relates to a graphite-based flame retardant, a graphite-based flame retardant finishing liquid, a preparation method and application thereof.
Background
The nylon 6 fabric is light, soft, high in strength and wear-resistant, and is widely applied to the fields of textile clothing, aerospace, building construction and the like, but the nylon 6 fabric has obvious inflammable defects, has high burning speed and is accompanied with serious molten drop behaviors. The flame-retardant and anti-dripping performance of the nylon 6 fabric is improved.
Conventional fabric flame retardants include halogen flame retardants, phosphorus flame retardants and the like, but the use of the halogen flame retardants is gradually forbidden due to the gradual increase of environmental protection requirements, and the phosphorus flame retardants are easy to cause eutrophication of water bodies and are also greatly limited in application to printing and dyeing enterprises. To address this problem, halogen-free and phosphorus-free flame retardant systems have been developed.
The expandable graphite is a common halogen-free and phosphorus-free flame retardant, the initial expansion temperature of the expandable graphite is 290-300 ℃, the expansion volume is more than or equal to 230ml/g, the expandable graphite can be instantaneously expanded by 150-300 times when meeting high temperature, and the expandable graphite is changed from a sheet shape into a worm shape, so that the structure is loose, porous and bent, the surface area is also enlarged, and the special structure has a good combustion-resisting effect. However, expandable graphite is poorly dispersible in aqueous solutions due to poor water solubility, thereby affecting its affinity for composites and textiles. This poor affinity directly results in the lack of flame retardant and water wash resistance properties of the expandable graphite modified textiles. This property therefore becomes a major obstacle to expandable graphite in composite and textile flame retardant modification applications.
Patent application CN111675881A discloses a preparation method of a dopamine surface functionalized expandable graphite flame-retardant epoxy resin, which adopts a dopamine oxidation self-polymerization technology to perform surface functionalization on expandable graphite to prepare the dopamine surface functionalized expandable graphite, and applies the dopamine surface functionalized expandable graphite to the epoxy resin, and active groups of the dopamine surface functionalized expandable graphite can be chemically bonded with epoxy groups of the epoxy resin, so that the stability and compatibility of the expandable graphite in the epoxy resin are improved. If the dopamine surface functionalized expandable graphite in the patent is applied to flame-retardant finishing of nylon 6 fabric, the water solubility of the dopamine surface functionalized expandable graphite is still poor, the dispersibility in aqueous solution is poor, and the affinity with the nylon 6 fabric is low, so that the performance of the nylon 6 fabric after flame-retardant finishing is still unsatisfactory.
Therefore, there is a great need to develop a graphite-based flame retardant with good water solubility and use it for flame-retardant finishing nylon 6 fabrics.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a graphite-based flame retardant, a graphite-based flame retardant finishing liquid, a preparation method and application thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a graphite-based flame retardant finishing liquid comprises the following steps:
(1) Preparing a reaction system a which contains expandable graphite, dopamine hydrochloride, hydrogen peroxide and a solvent and has a pH value of more than 7 (which can be adjusted by adding sodium hydroxide), and then reacting for 1-2 hours at 70-80 ℃;
(2) And adding glucose into the reaction system a to obtain a reaction system b, and reacting at 80-90 ℃ to obtain the graphite-based flame retardant finishing liquid.
In the step (1), under alkaline conditions (pH value is more than 7), a catalyst (hydrogen peroxide), high temperature (70-80 ℃) and short time (1-2 hours), only one part of dopamine hydrochloride in the reaction system a is subjected to self-polymerization to generate polydopamine, the polydopamine is coated on the surface of expandable graphite, and the other part of dopamine hydrochloride is in a free state;
in the step (2), maillard reaction occurs between glucose and polydopamine at 80-90 ℃, maillard reaction occurs between glucose and unreacted dopamine hydrochloride, dopamine hydrochloride self-aggregates, and polymerization reaction occurs between polydopamine and dopamine hydrochloride, and Maillard products and polydopamine are generated in the process, so that polydopamine and chain segments of the Maillard products are mutually interpenetrated and crosslinked, are tightly combined, and have no obvious interface problem.
If the dopamine hydrochloride in the step (1) is completely polymerized, the Maillard reaction in the step (2) is carried out, and the expandable graphite can be coated and modified, but the binding force between the Maillard product and the polydopamine is weaker, so that the washing resistance of the textile after flame-retardant finishing is poor.
The polydopamine has high adhesiveness, can be used for adhesion modification of any substance, however, although polydopamine has certain water solubility, the problem of poor water solubility of the expandable graphite cannot be solved, the Maillard product is a substance with high water solubility, the water solubility of the expandable graphite can be improved, however, the adhesion performance of the Maillard product to the expandable graphite is slightly poor, so that the effect of directly modifying the expandable graphite is poor, and therefore, the invention adopts polydopamine and the Maillard product to modify the expandable graphite.
As a preferable technical scheme:
according to the preparation method of the graphite-based flame retardant finishing liquid, in the step (1), the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 10-20:2-4:5-10, and the content of the expandable graphite in the reaction system a is 10-20 g/L.
According to the preparation method of the graphite-based flame retardant finishing liquid, in the step (1), the pH value of the reaction system a is 10-11.
According to the preparation method of the graphite-based flame retardant finishing liquid, in the step (2), the content of glucose in the reaction system b is 5-10 g/L, and the reaction time is 2-3 h.
The graphite-based flame retardant finishing liquid is prepared by adopting the preparation method of the graphite-based flame retardant finishing liquid.
The preparation method of the graphite-based flame retardant comprises the step of purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
A graphite-based flame retardant is prepared by adopting the preparation method of the graphite-based flame retardant.
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the steps of adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid, reacting at 80-90 ℃, and performing post-treatment (taking out, washing and drying) to obtain the halogen-free phosphorus-free flame-retardant nylon 6 fabric, wherein in the process, polydopamine and Maillard products in the graphite-based flame retardant finishing liquid are adhered to the nylon 6 fabric by virtue of higher adhesive property, and on the other hand, the polydopamine and Maillard products are subjected to covalent reaction with amino groups of polyamide 6 fibers to be grafted on the nylon 6 fabric.
As a preferable technical scheme:
According to the preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric, the bath ratio of the nylon 6 fabric to the graphite-based flame retardant finishing liquid is 1:30-50, and the reaction time is 1.5-2 hours.
The halogen-free and phosphorus-free flame-retardant nylon 6 fabric is prepared by adopting the preparation method of the halogen-free and phosphorus-free flame-retardant nylon 6 fabric.
The halogen-free phosphorus-free flame-retardant nylon 6 fabric has the advantages that the limiting oxygen index of the halogen-free phosphorus-free flame-retardant nylon 6 fabric is not lower than 28.3%, the damage length is not higher than 12.3cm, no molten drops are generated, the damage length is still lower than 14.5cm after 20 times of washing, no molten drops are generated, and the halogen-free phosphorus-free flame-retardant nylon 6 fabric has good flame-retardant molten drop-preventing performance and water-washing-resisting performance, because the polysaccharide ring of the Maillard product is decomposed into carbon at a lower temperature, the carbon is favorable for inhibiting molten drops of the nylon 6 fabric, however, the stability of carbon residues is poor, the expandable graphite has strong expansion capability, and the thermal stability and strength of carbon residues generated by the Maillard product are improved, so that the molten drops of the nylon 6 fabric are effectively inhibited, and the flame-retardant effect is achieved.
The beneficial effects are that:
(1) The invention adopts the polydopamine and the Maillard product to modify the expandable graphite, improves the water solubility of the expandable graphite, so that the expandable graphite can be uniformly dispersed on the surface of the nylon 6 fabric, the Maillard product on the surface of the modified expandable graphite contains active groups such as aldehyde groups, carboxyl groups and the like, and can be subjected to covalent bond bonding and ionic bond bonding with the nylon 6 fabric, so that the modified nylon 6 fabric has good washing resistance and durable flame retardant function;
(2) The invention adopts the expandable graphite, the expandable graphite has stronger expansion capability, and the heat stability and strength of carbon residue generated by Maillard products are improved, thereby effectively inhibiting the molten drop of nylon 6 fabrics and playing a better flame-retardant effect.
Drawings
FIG. 1 is a surface topography of a halogen-free and phosphorus-free flame retardant nylon 6 fabric prepared in example 8 of the invention.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples and comparative examples were examined for the relevant performance index:
The limiting oxygen index of the fabric was tested with reference to the standard of GB/T5454-1997 Experimental oxygen index for Combustion Performance of textiles.
The damage length and the occurrence of the molten drops are measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of the damage length of the vertical direction of the burning performance of the textile, and the occurrence of the molten drops is observed in the test process.
The damage length after 20 times of water washing and the generation of the molten drops are carried out, namely, the fabric is firstly washed for 20 times by referring to the standard of the accelerated test of the washing fastness of household and commercial use of AATCC 61-2013, and then the damage length of the fabric is tested by referring to the standard of the test of the smoldering and continuous burning time of the damage length of the burning performance of the textile in the vertical direction of GB/T5455-2014, and the generation of the molten drops is observed in the test process.
Example 1
A preparation method of a graphite-based flame retardant finishing liquid comprises the following specific steps:
(1) Raw material preparation:
The expandable graphite is manufactured by Shanghai Ala Latin Biochemical technology Co., ltd, and has the model E477901 and the initial expansion temperature of 290-300 ℃;
Dopamine hydrochloride;
Hydrogen peroxide;
Sodium hydroxide;
Solvent, namely water;
Glucose;
(2) Preparing a graphite-based flame retardant finishing liquid:
(2.1) preparing a reaction system a consisting of expandable graphite, dopamine hydrochloride, hydrogen peroxide, sodium hydroxide and a solvent, and then reacting for 2 hours at 70 ℃;
In the reaction system a, the pH value is 10, the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 10:2:05, and the content of the expandable graphite is 10g/L;
(2.2) adding glucose into the reaction system a to obtain a reaction system b with the glucose content of 5g/L, and then reacting for 3 hours at 80 ℃ to obtain a graphite-based flame retardant finishing liquid, and purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
Example 2
A preparation method of a graphite-based flame retardant finishing liquid comprises the following specific steps:
(1) Raw material preparation:
The expandable graphite is manufactured by Shanghai Ala Latin Biochemical technology Co., ltd, and has the model E477901 and the initial expansion temperature of 290-300 ℃;
Dopamine hydrochloride;
Hydrogen peroxide;
Sodium hydroxide;
Solvent, namely water;
Glucose;
(2) Preparing a graphite-based flame retardant finishing liquid:
(2.1) preparing a reaction system a consisting of expandable graphite, dopamine hydrochloride, hydrogen peroxide, sodium hydroxide and a solvent, and then reacting for 1.8 hours at 72 ℃;
In the reaction system a, the pH value is 10.5, the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 13:2.5:7, and the content of the expandable graphite is 13g/L;
(2.2) adding glucose into the reaction system a to obtain a reaction system b with the glucose content of 6g/L, and reacting at 83 ℃ for 2.7h to obtain a graphite-based flame retardant finishing liquid, and purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
Example 3
A preparation method of a graphite-based flame retardant finishing liquid comprises the following specific steps:
(1) Raw material preparation:
The expandable graphite is manufactured by Shanghai Ala Latin Biochemical technology Co., ltd, and has the model E477901 and the initial expansion temperature of 290-300 ℃;
Dopamine hydrochloride;
Hydrogen peroxide;
Sodium hydroxide;
Solvent, namely water;
Glucose;
(2) Preparing a graphite-based flame retardant finishing liquid:
(2.1) preparing a reaction system a consisting of expandable graphite, dopamine hydrochloride, hydrogen peroxide, sodium hydroxide and a solvent, and then reacting at 75 ℃ for 1.5h;
In the reaction system a, the pH value is 11, the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 15:4:8, and the content of the expandable graphite is 15g/L;
(2.2) adding glucose into the reaction system a to obtain a reaction system b with the glucose content of 7g/L, and reacting at 85 ℃ for 2.5h to obtain a graphite-based flame retardant finishing liquid, and purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
Example 4
A preparation method of a graphite-based flame retardant finishing liquid comprises the following specific steps:
(1) Raw material preparation:
The expandable graphite is manufactured by Shanghai Ala Latin Biochemical technology Co., ltd, and has the model E477901 and the initial expansion temperature of 290-300 ℃;
Dopamine hydrochloride;
Hydrogen peroxide;
Sodium hydroxide;
Solvent, namely water;
Glucose;
(2) Preparing a graphite-based flame retardant finishing liquid:
(2.1) preparing a reaction system a consisting of expandable graphite, dopamine hydrochloride, hydrogen peroxide, sodium hydroxide and a solvent, and then reacting for 1.3 hours at 77 ℃;
In the reaction system a, the pH value is 10.5, the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 18:3:8, and the content of the expandable graphite is 18g/L;
(2.2) adding glucose into the reaction system a to obtain a reaction system b with the glucose content of 9g/L, and reacting at 88 ℃ for 2.3 hours to obtain a graphite-based flame retardant finishing liquid, and purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
Example 5
A preparation method of a graphite-based flame retardant finishing liquid comprises the following specific steps:
(1) Raw material preparation:
The expandable graphite is manufactured by Shanghai Ala Latin Biochemical technology Co., ltd, and has the model E477901 and the initial expansion temperature of 290-300 ℃;
Dopamine hydrochloride;
Hydrogen peroxide;
Sodium hydroxide;
Solvent, namely water;
Glucose;
(2) Preparing a graphite-based flame retardant finishing liquid:
(2.1) preparing a reaction system a consisting of expandable graphite, dopamine hydrochloride, hydrogen peroxide, sodium hydroxide and a solvent, and then reacting for 1h at 80 ℃;
In the reaction system a, the pH value is 10, the weight ratio of the expandable graphite to the dopamine hydrochloride to the glucose is 20:3:10, and the content of the expandable graphite is 20g/L;
(2.2) adding glucose into the reaction system a to obtain a reaction system b with the glucose content of 10g/L, and then reacting for 2 hours at 90 ℃ to obtain a graphite-based flame retardant finishing liquid, and purifying the graphite-based flame retardant finishing liquid to obtain the graphite-based flame retardant.
Comparative example 1
A preparation method of a graphite-based flame retardant finishing liquid is basically the same as that in example 5, except that the reaction temperature in step (2.1) is 90 ℃ and the reaction time is 5 hours, and the dopamine hydrochloride in the system a is completely polymerized due to the excessively high reaction temperature and excessively long reaction time in the comparative example.
Example 6
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the following specific steps:
(1) Raw material preparation:
nylon 6 fabric with limiting oxygen index of 20.1% and damage length of 30cm;
the graphite-based flame retardant finishing liquid prepared in example 1;
(2) Preparing a flame-retardant nylon 6 fabric:
Adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid according to the bath ratio of 1:30, reacting for 2 hours at 80 ℃, taking out, washing and drying to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric.
The ultimate oxygen index of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is 28.3%, the damage length is 12.3cm, no molten drops are generated, the damage length is 14.5cm after 20 times of washing, and no molten drops are generated.
Example 7
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the following specific steps:
(1) Raw material preparation:
nylon 6 fabric with limiting oxygen index of 20.1% and damage length of 30cm;
the graphite-based flame retardant finishing liquid prepared in example 2;
(2) Preparing a flame-retardant nylon 6 fabric:
Adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid according to the bath ratio of 1:50, reacting for 1.8 hours at 82 ℃, taking out, washing and drying to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric.
The ultimate oxygen index of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is 29.5%, the damage length is 11.2cm, no molten drops are generated, the damage length is 13.9cm after 20 times of washing, and no molten drops are generated.
Example 8
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the following specific steps:
(1) Raw material preparation:
nylon 6 fabric with limiting oxygen index of 20.1% and damage length of 30cm;
the graphite-based flame retardant finishing liquid prepared in example 3;
(2) Preparing a flame-retardant nylon 6 fabric:
Adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid according to the bath ratio of 1:40, reacting for 1.5 hours at the temperature of 85 ℃, taking out, washing and drying to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric.
The surface morphology of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is shown in figure 1, the limiting oxygen index of the halogen-free phosphorus-free flame-retardant nylon 6 fabric is 30.3%, the damage length is 10.3cm, no molten drops are generated, the damage length is 13.3cm after 20 times of washing, and no molten drops are generated.
Example 9
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the following specific steps:
(1) Raw material preparation:
nylon 6 fabric with limiting oxygen index of 20.1% and damage length of 30cm;
the graphite-based flame retardant finishing liquid prepared in example 4;
(2) Preparing a flame-retardant nylon 6 fabric:
Adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid according to the bath ratio of 1:50, reacting for 1.2 hours at 87 ℃, taking out, washing and drying to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric.
The ultimate oxygen index of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is 31.2%, the damage length is 9.5cm, no molten drops are generated, the damage length is 12.7cm after 20 times of washing, and no molten drops are generated.
Example 10
The preparation method of the halogen-free phosphorus-free flame-retardant nylon 6 fabric comprises the following specific steps:
(1) Raw material preparation:
nylon 6 fabric with limiting oxygen index of 20.1% and damage length of 30cm;
the graphite-based flame retardant finishing liquid prepared in example 5;
(2) Preparing a flame-retardant nylon 6 fabric:
Adding the nylon 6 fabric into the graphite-based flame retardant finishing liquid according to the bath ratio of 1:50, reacting for 1h at 90 ℃, taking out, washing and drying to obtain the halogen-free and phosphorus-free flame retardant nylon 6 fabric.
The ultimate oxygen index of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is 32%, the damage length is 9.1cm, no molten drops are generated, the damage length is 12.4cm after 20 times of washing, and no molten drops are generated.
Comparative example 2
A preparation method of a halogen-free phosphorus-free flame retardant nylon 6 fabric is basically the same as that of example 10, except that the graphite-based flame retardant finishing liquid used in this comparative example is prepared from comparative example 1.
The ultimate oxygen index of the finally prepared halogen-free phosphorus-free flame-retardant nylon 6 fabric is 30.5%, the damage length is 10.3cm, no molten drops are generated, the damage length is 30cm after 20 times of washing, and the molten drops are generated.
Compared with the example 10, the halogen-free phosphorus-free flame retardant nylon 6 fabric prepared in the comparative example 2 has slightly poorer flame retardant performance before washing than the example 10, and the flame retardant performance after washing for 20 times is obviously deteriorated, because the graphite-based flame retardant finishing liquid prepared in the comparative example 1 used in the comparative example 2 has the advantages that dopamine hydrochloride is subjected to Maillard reaction after being completely polymerized in the preparation process, and expandable graphite can be coated and modified, but the binding force between Maillard products and polydopamine is weaker, so that the washing resistance of the textile after flame retardant finishing is poor.
Claims (9)
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| CN106280091A (en) * | 2016-08-12 | 2017-01-04 | 滁州市宏源喷涂有限公司 | High heat-resistant PVC NBR composite foamed plate that a kind of poly-dopamine film cladding is expanded graphite modified and preparation method thereof |
| CN111187518A (en) * | 2020-03-27 | 2020-05-22 | 蒋文彬 | Flame-retardant modified asphalt material and preparation process thereof |
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| CN106752681B (en) * | 2016-11-23 | 2019-05-14 | 厦门大学 | A kind of Water-borne inflation type refractory coating and preparation method thereof based on modified graphene oxide |
| CN111675881B (en) * | 2020-05-25 | 2022-04-29 | 南京工业大学 | A kind of preparation method of dopamine surface functionalized expandable graphite flame retardant epoxy resin |
| CN117362834B (en) * | 2023-11-08 | 2024-04-12 | 东莞市冠一塑料容器有限公司 | Antibacterial flame-retardant plastic, preparation method thereof and prepared food bottle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106280091A (en) * | 2016-08-12 | 2017-01-04 | 滁州市宏源喷涂有限公司 | High heat-resistant PVC NBR composite foamed plate that a kind of poly-dopamine film cladding is expanded graphite modified and preparation method thereof |
| CN111187518A (en) * | 2020-03-27 | 2020-05-22 | 蒋文彬 | Flame-retardant modified asphalt material and preparation process thereof |
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