CN104911910A - Preparation method of cellulose fabric having antibacterial and inflaming-retarding functions - Google Patents

Abstract

The invention relates to a method for preparing a cellulose fabric with antibacterial and flame-retardant functions, which belongs to the field of textile production. The method is to dissolve chitosan phosphate in butane tetracarboxylic acid solution, and add a catalytic amount to the solution. Sodium hypophosphite to configure fabric treatment solution, then soak the cellulose fabric in the fabric treatment solution, take it out and dry it. The technical scheme uses sodium hypophosphite as a catalyst, dissolves chitosan phosphate into butane tetracarboxylic acid to make a fabric treatment solution, then immerses the cellulose fabric in the fabric treatment solution, takes it out and rolls it dry to make the cellulose fabric both It has antibacterial and flame retardant functions, and the beneficial effect is remarkable.

Description

A kind of preparation method of cellulose fabric with antibacterial and flame retardant functions

technical field

The invention relates to a preparation method of a cellulose fabric with antibacterial and flame-retardant functions, belonging to the field of textile production.

Background technique

The application fields of fabrics are extremely wide, such as clothing fabrics, decorative fabrics, automotive fabrics, industrial fabrics, medical fabrics and aerospace military fabrics, etc., which are widely used in various fields related to the national economy and people's livelihood. Due to the low thermal stability of cellulose fibers , at 300°C to 400°C, it can be dehydrated to produce aliphatic and depolymerized to produce levoglucosan and then pyrolyzed. Levoglucosan decomposition products have high flammability and low molecular weight, and the oxidation heat can support the further development of cellulose. Pyrolysis.

Moreover, because the application of fabrics is closely related to people's daily life, and it is common for wearable products to come into contact with the skin, people have higher and higher requirements for the antibacterial properties of fabrics. Nowadays, fabrics have begun to appear on the market. Some fabrics with antibacterial function have been proposed, but because the fabric itself is easy to absorb and breed bacteria and fungal microorganisms, especially in underwear and medical fabrics, if the antibacterial effect is not good, it will greatly affect personal health, so it can be improved. The flammable properties of pre-cellulose fibers and the cellulose fabrics with antibacterial properties have become a research hotspot in this field.

Contents of the invention

Aiming at the deficiencies in the prior art, the present invention provides a method for preparing a cellulose fabric with both antibacterial and flame-retardant functions. The specific technical scheme is as follows:

A method for preparing cellulose fabrics with both antibacterial and flame-retardant functions, first dissolving chitosan phosphate in butane tetracarboxylic acid solution, adding a catalytic amount of sodium hypophosphite to the solution to prepare a fabric treatment solution, and then dissolving The cellulose fabric is soaked in the fabric treatment solution, taken out and rolled dry.

As an improvement of the above technical solution, the chitosan phosphate concentration is 2% to 6%, the butane tetracarboxylic acid concentration is 2% to 8%, and the sodium hypophosphite concentration is 2% to 8%.

As the improvement of above-mentioned technical scheme, described chitosan phosphate is according to following parts by weight:

Chitosan 15-30 parts

Urea 20-60 parts

Phosphoric acid 60～90 parts

Dimethylformamide 300～360 parts

Prepare by mixing, place at 95°C-105°C for 4h-6h, then filter, then wash with 50% (w/w) isopropanol aqueous solution for 3-4 times, and dry at 55°C-65°C.

As an improvement of the above technical solution, the fiber fabric is treated at 80° C. to 90° C. for 3 minutes to 5 minutes after drying, and then treated at 150° C. to 170° C. for 2 minutes to 3 minutes to further remove water.

As an improvement of the above technical solution, it is characterized in that the cellulose fabric is cotton fabric or linen fabric.

The above technical scheme uses sodium hypophosphite as a catalyst, dissolves chitosan phosphate into butane tetracarboxylic acid to make a fabric treatment solution, then immerses the cellulose fabric in the fabric treatment solution, takes it out and rolls it dry, so that the cellulose fabric can also It has antibacterial and flame retardant functions, and the beneficial effect is remarkable.

Instructions attached

Fig. 1 is the LOI value of the chitosan phosphate of embodiment four to eight different concentrations of the present invention;

Fig. 2 is the size of the inhibition zone of chitosan phosphate with different concentrations in Examples 4 to 8 of the present invention.

Detailed ways

The invention provides a preparation method of cellulose fabric with both antibacterial and flame-retardant functions. In the method, firstly, chitosan phosphate is dissolved in butane tetracarboxylic acid solution, and a catalytic amount of sodium hypophosphite is added to the solution to configure Fabric treatment solution, then soak the cellulose fabric in the fabric treatment solution, take it out and roll it dry. Further, the fiber fabric is treated at 80° C. to 90° C. for 3 minutes to 5 minutes to remove water after being rolled dry, and then treated at 150° C. to 170° C. for 2 minutes to 3 minutes to remove water.

Chitosan, a natural polysaccharide in the form of deacetylation, mainly exists in the exoskeleton chitin of crustaceans. Due to its multifunctionality, biodegradability and antibacterial properties, chitosan is often used as a An antibacterial agent, it will lose antibacterial activity due to the loss of cations under alkaline conditions, and poor durability due to poor adhesion to fabrics, and modified chitosan can overcome these problems. The present invention makes phosphate by chitosan, and this organophosphate can catalyze the formation of fat and depolymerization process L-glucose of cellulose, because the N-methylol group of organophosphorus compound can be combined with fiber The hydroxyl group of the cellulose fiber undergoes a condensation reaction to form a covalent bond, which can significantly improve the flame retardancy and surface adhesion of the fiber; butane tetracarboxylic acid is the most effective cross-linking agent, which can make the cellulose fiber have a good crease Restoration: sodium hypophosphite acts as a catalyst to catalyze the reaction.

Further, the concentration of the above-mentioned chitosan phosphate is 2% to 6%, the concentration of butane tetracarboxylic acid is 2% to 8%, and the concentration of sodium hypophosphite is 2% to 8%. Further, the concentration of chitosan phosphate is according to Following parts by weight:

Chitosan 15-30 parts

Urea 20-60 parts

Phosphoric acid 60～90 parts

Dimethylformamide 300～360 parts

Prepare by mixing, place at 95°C-105°C for 4h-6h, then filter, then wash with 50% (w/w) isopropanol aqueous solution for 3-4 times, and dry at 55°C-65°C.

In the above embodiments, the cellulose fabric may be any product made by weaving fibers, such as cotton fabric or linen fabric.

Embodiment one

Chitosan phosphate is according to following parts by weight:

Chitosan 15 parts

Urea 20 parts

Phosphoric acid 90 parts

Dimethylformamide 360 parts

Mix and prepare, place at 95°C for 4 hours, filter, then wash with 50% (w/w) isopropanol aqueous solution for 3 times, and dry at 55°C;

Then dissolve chitosan phosphate with a concentration of 2% in a solution of 2% butane tetracarboxylic acid, add sodium hypophosphite with a concentration of 2% to the solution to prepare a fabric treatment solution, and then immerse the cotton fabric in the fabric treatment solution and take it out Afterwards, it was rolled dry, treated at 80°C for 3 minutes to remove water, and then treated at 150°C for 2 minutes to further remove water.

The cotton fabrics prepared above were subjected to limiting oxygen index measurement and antibacterial test respectively, compared with cotton fabrics treated with chitosan phosphate, and compared the flame retardancy and antibacterial properties of the method provided by the invention. Wherein the flame retardancy is characterized by the limiting oxygen index LOI, and the higher the LOI, the less flammable the material is; wherein the antibacterial property is by placing the cotton fabric processed by the method of the present invention on Candida albicans, Staphylococcus aureus, In the colonies of Escherichia coli, the inhibition zone was recorded. The experimental data of its flame retardant and antibacterial properties are shown in Table 1 below:

Table 1 embodiment one flame retardant, antibacterial experimental data

Through the experimental data, it can be found that the flame retardancy and antibacterial properties of cotton fabrics are enhanced.

Embodiment two

Chitosan phosphate is according to following parts by weight:

Chitosan 30 parts

Urea 60 parts

Phosphoric acid 60 parts

Dimethylformamide 300 parts

Prepare by mixing, place at 105°C for 6 hours, filter, then wash 4 times with 50% (w/w) isopropanol aqueous solution, and dry at 65°C;

Then dissolve chitosan phosphate with a concentration of 6% in a solution of 8% butane tetracarboxylic acid, add sodium hypophosphite with a concentration of 8% to the solution to prepare a fabric treatment solution, and then immerse the cotton fabric in the fabric treatment solution and take it out Afterwards, it was rolled dry, treated at 90°C for 5 minutes to remove water, and then treated at 170°C for 3 minutes to further remove water.

The above-mentioned cotton fabrics were carried out to measure the limiting oxygen index respectively, and carried out the antibacterial test, compared with the cotton fabrics without adding chitosan phosphate treatment, its flame retardant, antibacterial experimental data are shown in the following table 2:

Table 2 embodiment two flame retardant, antibacterial experimental data

Through the experimental data, it can be found that the flame retardancy and antibacterial properties of cotton fabrics are greatly enhanced.

Embodiment three

Chitosan phosphate is according to following parts by weight:

Chitosan 23 parts

Urea 40 parts

Phosphoric acid 75 parts

Dimethylformamide 332 parts

Mix and prepare, place at 100°C for 5 hours, filter, then wash with 50% (w/w) isopropanol aqueous solution for 4 times, and dry at 60°C;

Then dissolve chitosan phosphate with a concentration of 2% in a solution of 6% butane tetracarboxylic acid, add sodium hypophosphite with a concentration of 6% to the solution to prepare a fabric treatment solution, and then immerse the linen fabric in the fabric treatment solution and take it out Afterwards, it was dried by rolling, treated at 85°C for 3 minutes to remove water, and then treated at 160°C for 2 minutes to further remove water.

The flax fabrics prepared above were measured for limiting oxygen index respectively, and antibacterial test was carried out, compared with the flax fabrics treated with chitosan phosphate, its flame retardant, antibacterial experimental data are shown in the following table 3:

Table 3 embodiment two flame retardant, antibacterial experimental data

The difference between this embodiment and Embodiments 1 and 2 is that flax fabrics are used for flame retardancy and antibacterial experiments, and it can be found from the experimental data that the flame retardancy and antibacterial properties of flax fabrics are enhanced.

Embodiment four to eight

Through five groups of experiments, the effects of different concentrations of chitosan phosphate on the flame retardancy and antibacterial properties of cellulose fabrics were tested. A group of control groups were set up in the experiment. The specific experimental steps are as follows:

Chitosan phosphate is according to following parts by weight:

Chitosan 23 parts

Urea 40 parts

Phosphoric acid 75 parts

Dimethylformamide 332 parts

Mix and prepare, place at 100°C for 5 hours, filter, then wash with 50% (w/w) isopropanol aqueous solution for 4 times, and dry at 60°C;

Then the chitosan phosphate that concentration is 2%, 3%, 4%, 5%, 6% is dissolved in concentration and is in 6% butane tetracarboxylic acid solution, and each concentration chitosan phosphate is respectively corresponding embodiment four , 5, 6, 7, 8, add 6% sodium hypophosphite to the solution to configure the fabric treatment solution, then immerse the cotton fabric in the fabric treatment solution, take it out and dry it, treat it at 85°C for 3 minutes to remove water, and then dry it at 160°C °C for 2 min to further remove water.

The above-mentioned cotton fabrics obtained were tested for limiting oxygen index and antibacterial test, compared with cotton fabrics treated with chitosan phosphate, the flame retardant and antibacterial test data are shown in Table 4 below:

Table 4 Flame retardant, antibacterial experimental data of embodiment four to eight

Through the experimental data, it can be found that with the increasing concentration of chitosan phosphate, the flame retardancy and antibacterial properties of cotton fabrics are gradually enhanced.

Claims (5)

1. a kind of preparation method of the cellulose fabric with antibacterial and flame retardant function concurrently is characterized in that, earlier chitosan phosphate is dissolved in butane tetracarboxylic acid solution, adds the sodium hypophosphite configuration of catalytic amount in the solution Fabric treatment solution, then soak the cellulose fabric in the fabric treatment solution, take it out and roll it dry. 2. a kind of preparation method of the cellulose fabric with antibacterial and flame-retardant function concurrently as claimed in claim 1, is characterized in that, described chitosan phosphate concentration is 2%～6%, and described butane four The concentration of carboxylic acid is 2%-8%, and the concentration of sodium hypophosphite is 2%-8%. 3. a kind of preparation method of the cellulose fabric with antibacterial and flame-retardant function concurrently as claimed in claim 2, is characterized in that, described chitosan phosphate is according to following parts by weight: Chitosan 15-30 parts Urea 20-60 parts Phosphoric acid 60～90 parts Dimethylformamide 300～360 parts Prepare by mixing, place at 95°C-105°C for 4h-6h, then filter, then wash with 50% (w/w) isopropanol aqueous solution for 3-4 times, and dry at 55°C-65°C. 4. A method for preparing a cellulose fabric with antibacterial and flame-retardant functions as claimed in claim 1, wherein the fiber fabric is dried at 80°C to 90°C for 3min to 5min to remove water , and then treated at 150°C to 170°C for 2min to 3min to further remove water. 5. The preparation method of a kind of cellulose fabric with antibacterial and flame-retardant functions as claimed in any one of claims 1-4, characterized in that, the cellulose fabric is cotton fabric or linen fabric.