Disclosure of Invention
The invention aims to provide a flame-retardant fabric and a preparation method thereof, the prepared flame-retardant compound can be mixed with graphene oxide to modify molten polypropylene to prepare modified polypropylene, and the flame-retardant fabric prepared with cotton fibers is soft and breathable, has an excellent flame-retardant effect and has a wide application prospect.
The technical scheme of the invention is realized as follows:
the invention provides a flame-retardant fabric which comprises a flame-retardant compound, graphene oxide, polypropylene and cotton fibers;
the flame retardant compound has a structure as shown in formula I:
as a further improvement of the invention, the invention is prepared from the following raw materials in parts by weight: 3-5 parts of flame retardant compound, 2-4 parts of graphene oxide, 40-60 parts of polypropylene and 30-40 parts of cotton fiber.
As a further improvement of the present invention, the method for synthesizing the flame retardant compound is as follows: and (3) heating phytic acid and ethylenediamine to react under the action of a catalyst to obtain the flame-retardant compound.
As a further improvement of the present invention, the catalyst is phosphorus trichloride.
As a further improvement of the invention, the mol ratio of the phytic acid to the ethylenediamine is 1:12-12.5, and the mass of the catalyst is 5-10wt% of the phytic acid.
As a further improvement of the invention, the heating temperature is 80-90 ℃ and the time is 3-4h.
As a further improvement of the present invention, the method for synthesizing the flame retardant compound is as follows: adding 1 molar equivalent of phytic acid and 12-12.5 molar equivalents of ethylenediamine into DMF, adding phosphorus trichloride accounting for 5-10wt% of phytic acid, stirring and mixing uniformly, heating to 80-90 ℃, stirring and reacting for 3-4h, adding equal volume of saturated sodium bicarbonate, filtering, washing and drying to obtain the flame-retardant compound.
The invention further provides a preparation method of the flame-retardant fabric, which comprises the following steps:
s1, heating and melting polypropylene, adding a flame retardant compound and graphene oxide, stirring and mixing uniformly, and spinning to obtain modified polypropylene fibers;
s2, preparing the modified polypropylene fibers and the cotton fibers into yarns according to a proportion, and drying and spinning to obtain the flame-retardant fabric.
As a further improvement of the invention, the temperature of the heating and melting is 140-160 ℃.
The invention has the following beneficial effects: the organic phosphorus-nitrogen flame retardant has the advantages of no toxicity, no smell, high heat stability, good flame retardant effect, low cost and the like, can be decomposed to generate inert nitrogen-containing gas (such as ammonia gas) after being heated, dilutes the concentration of combustible gas and oxygen in a combustion area, prevents continuous combustion, has good flame retardant effect, contains high proportion of phosphorus and nitrogen elements, has good flame retardant effect, is simple in preparation method, mild in synthesis condition and high in yield, has the characteristic of high temperature resistance, can be mixed with graphene oxide to modify molten polypropylene, and can be used for preparing modified polypropylene, and the flame retardant fabric prepared with cotton fibers is soft and breathable, has excellent flame retardant effect and has wide application prospect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Preparation example 1 Synthesis of flame retardant Compound
As in fig. 1, the method is as follows:
0.1mol of phytic acid and 1.2mol of ethylenediamine are added into 200mL of DMF, phosphorus trichloride accounting for 5wt% of the phytic acid is added, stirring and mixing are carried out uniformly, heating is carried out to 80 ℃, stirring and reacting are carried out for 3 hours, equal volume of saturated sodium bicarbonate is added, filtering, washing and drying are carried out, and the flame retardant compound is prepared, and the yield is 89.5%.
Preparation example 2 Synthesis of flame retardant Compound
As in fig. 1, the method is as follows:
0.1mol of phytic acid and 1.25mol of ethylenediamine are added into 200mL of DMF, phosphorus trichloride accounting for 10wt% of the phytic acid is added, stirred and mixed uniformly, heated to 90 ℃, stirred and reacted for 4 hours, equal volume of saturated sodium bicarbonate is added, filtered, washed and dried, and the flame retardant compound is prepared, and the yield is 91.2%.
Preparation example 3 Synthesis of flame retardant Compound
As in fig. 1, the method is as follows:
0.1mol of phytic acid and 1.22mol of ethylenediamine are added into 200mL of DMF, 7wt% of phosphorus trichloride accounting for the phytic acid is added, stirred and mixed uniformly, heated to 85 ℃, stirred and reacted for 3.5h, equal volume of saturated sodium bicarbonate is added, filtered, washed and dried, and the flame retardant compound is prepared, and the yield is 90.7%.
Example 1
The raw materials comprise the following components in parts by weight: 3 parts of flame retardant compound prepared in preparation example 1, 2 parts of graphene oxide, 40 parts of polypropylene and 30 parts of cotton fiber.
The preparation method comprises the following steps:
s1, heating polypropylene to 140 ℃ for melting, adding a flame retardant compound and graphene oxide, stirring and mixing uniformly, and spinning to obtain modified polypropylene fibers;
s2, preparing the modified polypropylene fibers and the cotton fibers into yarns according to a proportion, and drying and spinning to obtain the flame-retardant fabric.
Example 2
The raw materials comprise the following components in parts by weight: 5 parts of flame retardant compound prepared in preparation example 2, 4 parts of graphene oxide, 60 parts of polypropylene and 40 parts of cotton fiber.
The preparation method comprises the following steps:
s1, heating polypropylene to 160 ℃ for melting, adding a flame retardant compound and graphene oxide, stirring and mixing uniformly, and spinning to obtain modified polypropylene fibers;
s2, preparing the modified polypropylene fibers and the cotton fibers into yarns according to a proportion, and drying and spinning to obtain the flame-retardant fabric.
Example 3
The raw materials comprise the following components in parts by weight: 4 parts of flame retardant compound prepared in preparation example 3, 3 parts of graphene oxide, 50 parts of polypropylene and 35 parts of cotton fiber.
The preparation method comprises the following steps:
s1, heating polypropylene to 150 ℃ for melting, adding a flame retardant compound and graphene oxide, stirring and mixing uniformly, and spinning to obtain modified polypropylene fibers;
s2, preparing the modified polypropylene fibers and the cotton fibers into yarns according to a proportion, and drying and spinning to obtain the flame-retardant fabric.
Comparative example 1
The difference compared to example 3 is that no flame retardant compound is added.
Comparative example 2
The difference from example 3 is that graphene oxide was not added.
Test example 1
The flame retardant fabrics prepared in examples 1-3 and comparative examples 1-2 of the present invention and commercially available flame retardant fabrics were subjected to performance tests, and the results are shown in Table 1.
Air permeability of the fabric: the fabric breathability was tested according to GB/T5453-1997 determination of breathability of textile fabrics, the test results being expressed in terms of air permeability.
Wear resistance of the fabric: the fabric was subjected to wear resistance testing according to astm d3884 wear test method, the results of which are expressed as wear resistance times.
TABLE 1
Group of
|
Air permeability (mm/s)
|
Wear-resisting times (times)
|
Example 1
|
95
|
7000
|
Example 2
|
96
|
7100
|
Example 3
|
96
|
7200
|
Comparative example 1
|
94
|
6700
|
Comparative example 2
|
92
|
5600
|
Commercially available flame-retardant fabric
|
85
|
5000 |
As can be seen from the above table, the flame retardant fabrics prepared in examples 1-3 of the present invention have good air permeability and wear resistance.
Test example 2
The flame retardant fabrics prepared in examples 1-3 and comparative examples 1-2 of the present invention and commercially available flame retardant fabrics were subjected to performance tests, and the results are shown in Table 3.
The testing method comprises the following steps: and (3) testing by adopting a vertical combustion experiment, wherein the continuous combustion time is tested: s, smoldering time: s, melting and dripping.
TABLE 3 Table 3
Group of
|
Testing the burn time(s)
|
Smoldering time(s)
|
Melting and dripping conditions
|
Example 1
|
0
|
0
|
Without any means for
|
Example 2
|
0
|
0
|
Without any means for
|
Example 3
|
0
|
0
|
Without any means for
|
Comparative example 1
|
5.2
|
7.8
|
Most of melting
|
Comparative example 2
|
2.1
|
3.2
|
Melting in a small amount
|
Commercially available flame-retardant fabric
|
2.9
|
4.0
|
Partial melting |
As can be seen from the above table, the flame-retardant fabrics prepared in examples 1 to 3 of the present invention have good flame-retardant effect.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.