Background
With the vigorous development of synthetic fiber materials and textile products thereof, the composite fiber materials rapidly replace traditional materials, are widely applied to various departments of national economy such as industry, agriculture, military and the like, and are closely related to daily life of people. However, these textiles have Limiting Oxygen Index (LOI) values below 26.0%, are extremely flammable in air, and sometimes produce dense smoke and toxic gases once burned, which pose a hazard to the environment and create a great potential for human life and property safety. Therefore, research and development of the flame retardant fabric has important practical significance for improving the use safety and expanding the application field of the flame retardant fabric. However, current flame retardant fabrics still face environmental-friendly limitations. Firstly, the most applied halogen-based and organic phosphorus-based flame retardants are used for flame-retardant finishing of fabrics, harmful substances and phosphorus-rich substances exist, the health of human beings and the ecological safety are seriously endangered, and secondly, the fabrics finished by the halogen-free, nontoxic and formaldehyde-free flame retardants have poor flame-retardant performance and cannot meet the requirement of industrialization. Therefore, how to realize the environment-friendly and good flame retardance of the fabric becomes a key problem to be solved urgently in the flame retardance field.
The lyocell fabric is woven by lyocell fibers, the lyocell fibers are called green fibers, the lyocell fibers have stable and excellent performance, the raw materials are nontoxic and harmless and are easy to obtain, the performance is superior to that of artificial synthetic fibers and natural fibers, and the whole production process can not generate pollution and toxic chemical reaction. Meanwhile, the fiber has high dry and wet strength, high swelling ratio, unique fibrillation characteristic and good spinnability. The lyocell fabric has a wide application range from clothing fabric to fabric products in the fields of industry, agriculture and military. However, the lyocell fabric belongs to inflammable fabrics like other synthetic fibers, which greatly limits the application field of the lyocell fabric. Therefore, imparting excellent flame retardancy to lyocell fabric is an important point of attention.
The inventor of the present application found in the research process that the existing flame-retardant lyocell has the problems of low cost, bio-based, washability and the like.
Disclosure of Invention
The invention aims to provide a bio-based durable flame-retardant lyocell fabric and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
A preparation method of a bio-based durable flame retardant lyocell fabric, which comprises the following steps:
s1, dissolving polyethyleneimine in a solvent I to prepare a solution I;
S2, dissolving phytic acid and chitosan in a second solvent to prepare a second mixed solution;
S3, immersing the lyocell fabric into the first solution and the second mixed solution in sequence for reaction, and carrying out padding, pre-drying and baking treatment on the lyocell fabric after each immersion in the first solution and the reaction are finished;
S4, repeating the operation S3, and padding and baking to obtain the bio-based durable flame-retardant lyocell fabric.
Preferably, the first solvent and the second solvent are deionized water.
Preferably, the first solution in the S1 is 0.5-3.0wt%.
Preferably, the mass fraction of the phytic acid in the S2 is 10-20%, the mass fraction of the chitosan is 2-4%, and the chitosan is mixed according to a ratio of 1:1 to prepare a mixed solution II with a ratio of 5.0-10.0% to 1.0-2.0%.
Preferably, the rolling rate in the step S3 is controlled to be 100% +/-10%, the pre-baking treatment temperature is 100 ℃, and the baking treatment temperature is 130 ℃.
Preferably, after finishing the secondary liquid rolling, pre-drying and baking treatment cycle in the step S3, the method uses deionized water for washing to remove unreacted substances.
Preferably, the bio-based durable flame-retardant lyocell fabric is prepared by the preparation method of the bio-based durable flame-retardant lyocell fabric.
Compared with the prior art, the invention has the beneficial effects that:
The invention adopts animal and plant extracted chitosan and phytic acid as main flame-retardant elements, and biodegradable polyethyleneimine as fiber protective agent and film-forming component, and prepares the bio-based washable flame-retardant lyocell fiber by a simple and environment-friendly method, and the prepared flame-retardant lyocell fiber has good flame-retardant performance, good washable performance and broad market prospect.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described 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.
Example 1:
referring to fig. 1, a preparation method of a bio-based durable flame retardant lyocell fabric comprises the following steps:
s1, dissolving polyethyleneimine in deionized water to prepare 1.0wt% solution I;
S2, mixing a certain amount of phytic acid with mass fraction of 10.0% and chitosan with mass fraction of 2.0% according to a ratio of 1:1 to prepare a mixed solution II with mass fraction of 5.0% to 1.0%;
s3, immersing the lyocell fabric into the first solution S1 to protect the lyocell fiber from acid damage to cellulose, simultaneously providing partial amino groups to react with unreacted phosphoric acid groups, and immersing the second mixed solution S2;
And S4, repeating the operation S3, and padding and baking to obtain the lyocell flame-retardant fabric.
And (3) carrying out padding, pre-drying and baking treatment on the lyocell fabric after each time of immersing in the solution and finishing the reaction in the step (S3), wherein the padding rate is controlled to be 100% +/-10%, the pre-drying treatment temperature is 100 ℃, the baking treatment temperature is 130 ℃, and after the secondary S3 circulation is finished, washing with deionized water to remove unreacted substances.
Phytic acid (PHYTIC ACID, abbreviated as PA), chitosan (chitosan, abbreviated as CH), and polyethylenimine (Poly (ethylenimine), abbreviated as PEI).
The added biodegradable polyethyleneimine is used as a fiber protective agent and a film forming component, and the flame retardant property of the bio-based modified lyocell fabric is obviously improved, the bio-based modified lyocell fabric has good washable property and less damage to the physical property of the lyocell fabric, and has very wide application prospect in the fields of textile, home furnishing and protective equipment.
Example 2:
referring to fig. 1, a preparation method of a bio-based durable flame retardant lyocell fabric comprises the following steps:
S1, dissolving polyethyleneimine in deionized water to prepare a solution I with the weight percent of 3.0;
S2, mixing a certain amount of phytic acid with mass fraction of 20.0% and chitosan with mass fraction of 4.0% according to a ratio of 1:1 to prepare a mixed solution II with mass fraction of 10.0% to 2.0%;
s3, immersing the lyocell fabric into the first solution S1 to protect the lyocell fiber from acid damage to cellulose, simultaneously providing partial amino groups to react with unreacted phosphoric acid groups, and immersing the second mixed solution S2;
And S4, repeating the operation S3, and padding and baking to obtain the lyocell flame-retardant fabric.
And (3) carrying out padding, pre-drying and baking treatment on the lyocell fabric after each time of immersing in the solution and finishing the reaction in the step (S3), wherein the padding rate is controlled to be 100% +/-10%, the pre-drying treatment temperature is 100 ℃, the baking treatment temperature is 130 ℃, and after the secondary S3 circulation is finished, washing with deionized water to remove unreacted substances.
Example 3:
referring to fig. 1, a preparation method of a bio-based durable flame retardant lyocell fabric comprises the following steps:
s1, dissolving polyethyleneimine in deionized water to prepare 0.5wt% solution I;
S2, mixing a certain amount of phytic acid with mass fraction of 10.0% and chitosan with mass fraction of 2.0% according to a ratio of 1:1 to prepare a mixed solution II with mass fraction of 5.0% to 1.0%;
s3, immersing the lyocell fabric into the first solution S1 to protect the lyocell fiber from acid damage to cellulose, simultaneously providing partial amino groups to react with unreacted phosphoric acid groups, and immersing the second mixed solution S2;
And S4, repeating the operation S3, and padding and baking to obtain the lyocell flame-retardant fabric.
And (3) carrying out padding, pre-drying and baking treatment on the lyocell fabric after each time of immersing in the solution and finishing the reaction in the step (S3), wherein the padding rate is controlled to be 100% +/-10%, the pre-drying treatment temperature is 100 ℃, the baking treatment temperature is 130 ℃, and after the secondary S3 circulation is finished, washing with deionized water to remove unreacted substances.
Characterization data and effect data for the products of the examples and comparative examples are shown in the following table:
the flame retardant effect of the lyocell fabric is shown in figure 2.
The untreated lyocell fabric had an as-received Limiting Oxygen Index (LOI) of 18.0% and was a flammable material, and the flame retardant sample of example 1 had an LOI of 34.5% far higher than the untreated lyocell fabric, reaching a flame retardant rating. In the vertical burning test, the original damaged charcoal is nearly the full length of the fabric, the continuous burning time is 8.0+/-0.5 s, the smoldering burning time is 125+/-5 s, the burning is intense and continuous smoldering, the fire risk is extremely high, the damaged charcoal of the flame-retardant sample of the embodiment 1 is only 50+/-5 mm, the continuous burning time and the smoldering time are 0s, the flame is quickly inhibited, the burning range is extremely small and no continuous burning exists, and the flame-retardant effect is excellent. The flame retardant sample of the embodiment 1 still maintains good flame retardant performance after 20 times of water washing, namely LOI is 26.3 percent after water washing, but is slightly reduced but still higher than a flame retardant critical value of 26 percent, flame retardant property is maintained, the carbon damage length is increased to 230+/-5 mm in a vertical combustion test, the continuous combustion time is only 2.0+/-0.5 s, no smoldering phenomenon exists, flame spreading can be effectively inhibited, continuous combustion is avoided, and good durability is reflected.
According to the invention, through the synergistic effect of the bio-based material (chitosan and phytic acid) and the polyethyleneimine, the flame retardant property of the lyocell fabric is remarkably improved, and the problem that the flame retardance and the washability are difficult to be compatible in the traditional flame retardant treatment is solved. The data show that the treated fabric has the flame retardant performance improved, the practical flame retardant effect is still maintained after 20 times of water washing, the used materials are all biological bases or degradable components, the environment is protected, the damage to the physical properties of the fabric is small, and a feasible scheme is provided for the safe application of the lyocell fabric in the fields of textile, home furnishings, protective equipment and the like.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.