CN117626632A - Self-cleaning textile fiber and preparation process thereof - Google Patents

Self-cleaning textile fiber and preparation process thereof Download PDF

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Publication number
CN117626632A
CN117626632A CN202311731376.5A CN202311731376A CN117626632A CN 117626632 A CN117626632 A CN 117626632A CN 202311731376 A CN202311731376 A CN 202311731376A CN 117626632 A CN117626632 A CN 117626632A
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self
fiber
tio
cleaning textile
acid
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CN202311731376.5A
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杨华伟
杨俊辉
任如同
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Funan County Shengqian Knitting Co ltd
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Funan County Shengqian Knitting Co ltd
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Abstract

The invention discloses a self-cleaning textile fiber and a preparation process thereof, and belongs to the technical field of textile fibers. The method comprises the steps of preparing modified titanium dioxide sol in advance, and immersing a nascent composite fiber obtained by melt mixing spinning of fiber and rosin into the titanium dioxide sol and a cross-linking agent to obtain the self-cleaning textile fiber. Compared with the traditional method, the textile fiber prepared by the method has excellent hydrophobic property and extremely strong self-cleaning capability, and the preparation process is simple, so that large-scale continuous production can be realized.

Description

Self-cleaning textile fiber and preparation process thereof
Technical Field
The invention belongs to the technical field of textile fibers, and particularly relates to a self-cleaning textile fiber and a preparation process thereof.
Background
Along with the improvement of living standard, the improvement of human body protection concept in professional work and the damage of external natural environment, people have new demands on the functionality of clothing and household textiles. The development of functional fibers is a substrate for preparing functional textiles, and functional fiber-based is one of the important ways to develop functional textiles. In recent years, research into self-cleaning functional fibers has become one of the hot problems of concern. The self-cleaning fiber is used in the textile field, can effectively shield and eliminate various environmental pollutants such as bacteria, viruses, pesticides, stains and the like, avoid the damage of the pollutants to human bodies through skin or respiratory tracts, and can effectively relieve the environmental and energy problems caused by washing and effectively protect the human bodies from being damaged by the environmental pollutants, so that the research and industrialization of the self-cleaning fiber and textiles have very important significance.
Nanometer TiO 2 Has the advantages of excellent photocatalytic property, stable chemical property, no secondary pollution and the like, is considered to be the green environment-friendly photocatalytic material with development prospect at present, and is nano TiO 2 The method has wide application in textile processing, plays an extremely critical role in preparing functional fabrics with the same functions of environmental purification, self-cleaning, antibacterial deodorization, super-hydrophobic and ultraviolet resistance, and has huge industrialization potential. Nanometer TiO 2 Hydrosol belongs to a thermodynamically stable system, has extremely high stability, is more suitable for being applied as a fabric finishing agent, does not need energy-consuming roasting or hydrothermal treatment, is energy-saving and environment-friendly, has lower cost, has bright application prospect, and has a plurality of problems as follows: in order to solve the problems, raw materials which are suitable for textiles, low in cost, environment-friendly and durable are required to be developed, the process is further simplified, and the reliability is improved.
Disclosure of Invention
The invention aims to provide a self-cleaning textile fiber and a preparation process thereof, which are used for solving the problems of insufficient adhesive force and easy falling of the textile fiber in a sol-gel method.
The aim of the invention can be achieved by the following technical scheme:
a preparation process of self-cleaning textile fibers specifically comprises the following steps:
step one: stearic acid and TiO 2 Adding into dimethylbenzene, stirring, centrifugally filtering, washing, drying and grinding to obtain stearic acid grafted TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Grafting stearic acidBranch TiO 2 Adding 4-vinylbenzoic acid and 4-vinylaniline into deionized water, performing ultrasonic dispersion, introducing nitrogen at room temperature for protection, adding an initiator for reaction, heating to 65-70 ℃ for reaction, alternately washing with anhydrous ethanol and water, and vacuum drying to obtain modified TiO 2
Step two: modified TiO 2 Adding the mixture into deionized water, stirring and carrying out ultrasonic treatment to obtain modified TiO 2 Sol;
step three: the fiber and rosin are mixed according to the mass ratio of 7-10:1-2, adding the mixture into a double-screw extruder, uniformly mixing, extruding composite master batch, putting the mixture into a drying oven for drying, adding the mixture into a spinning machine for melt blowing, drafting, degassing and drying, and collecting the mixture to obtain primary composite fibers;
step four: immersing the primary composite fiber obtained in the second step into the modified TiO obtained in the first step 2 And (3) adhering the sol and the cross-linking agent, stirring, and carrying out coagulating bath, ethanol washing and water washing, and airing to constant weight to obtain the self-cleaning textile fiber.
Further, the fibers include one of cotton fibers, flax fibers, regenerated cellulose fibers and bamboo charcoal fibers.
Further, the stearic acid is one of oleic acid, tetradecanoic acid and n-heptanoic acid.
Further, the initiator is one of potassium persulfate and ammonium persulfate.
Further, the cross-linking agent is one of butane tetracarboxylic acid, glutaraldehyde and succinic acid.
Further, stearic acid and TiO in the first step 2 And xylene in an amount ratio of 1.8 to 2.3g:2.2-2.5g:50mL; stearic acid grafted TiO 2 The dosage ratio of 4-vinylbenzoic acid, 4-vinylaniline, deionized water and initiator is 2g:2-4g:1-2g:400mL:0.3-0.5g; modified TiO in the second step 2 And deionized water in the amount of 5-8g:500mL.
Further, in the fourth step, the primary composite fiber and the modified TiO are prepared 2 The mass ratio of the sol to the cross-linking agent is 1:1.2-1.5:0.1-0.2.
A self-cleaning textile fiber is prepared by the steps.
The invention has the beneficial effects that:
in the invention, stearic acid is firstly used for grafting TiO 2 The nano particles reduce the surface energy, and then 4-vinylaniline and 4-vinylbenzoic acid are utilized to carry out in-situ polymerization under the action of an initiator, so that the TiO is improved 2 Dispersibility in nanoparticle sizes; and under the action of the cross-linking agent, the cohesiveness of the fiber and the modified silica gel solution is improved, so that the fiber and the modified silica gel solution can be firmly combined together, and the durability of the self-cleaning textile fiber is improved.
According to the invention, the rosin added in the self-cleaning textile fiber is effectively induced to refine the fiber through the osmosis, so that the average diameter of the fiber is reduced, the number of the fiber is increased, the textile fiber can have better hand feeling after application, is more exquisite, and the application field of the self-cleaning textile fiber is enlarged.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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
The preparation process of the self-cleaning textile fiber comprises the following specific steps:
step one: first 1.8g oleic acid and 2.2g TiO were added 2 Adding (50 nm) into 50mL of dimethylbenzene, stirring for 3h, centrifugally filtering, washing with ethanol solution for 3 times, drying at 60 ℃, grinding, and sieving with a 300-mesh sieve to obtain stearic acid grafted TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the 2g of stearic acid is grafted with TiO 2 Adding 4g of 4-vinylbenzoic acid and 1g of 4-vinylaniline into 400mL of deionized water, dispersing for 0.5h by ultrasonic, introducing nitrogen at room temperature for protection, adding 0.45g of potassium persulfate, reacting for 1h, heating to 65 ℃ for continuous reaction for 2h, alternately washing with absolute ethyl alcohol and water for 3 times, and drying in a vacuum box at 60 ℃ for 3h to obtain modified TiO 2
Step two: modified TiO 0.5g 2 Adding the mixture into 50mL of deionized water, magnetically stirring the mixture for 2 hours, and performing ultrasonic treatment for 2 hours to obtain modified TiO 2 Sol;
step three: adding 7g of cotton fiber and 2g of rosin into a double-screw extruder, uniformly mixing, extruding composite master batch, putting into an oven for drying, adding into a spinning machine for melt blowing, drafting, degassing and drying, and collecting to obtain primary composite fiber;
step four: immersing 1g of the primary composite fiber obtained in the second step into 1.3g of modified TiO obtained in the first step 2 The sol and 0.15g of butane tetracarboxylic acid are adhered, stirred uniformly, and dried to constant weight through coagulating bath, ethanol washing and water washing to obtain the self-cleaning textile fiber.
Example 2
The preparation process of the self-cleaning textile fiber comprises the following specific steps:
step one: first, 2.1g of tetradecanoic acid and 2.3g of TiO are reacted 2 Adding (50 nm) into 50mL of dimethylbenzene, stirring for 3h, centrifugally filtering, washing with ethanol solution for 3 times, drying at 60 ℃, grinding, and sieving with a 300-mesh sieve to obtain stearic acid grafted TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the 2g of stearic acid is grafted with TiO 2 Adding 3g of 4-vinylbenzoic acid and 1g of 4-vinylaniline into 400mL of deionized water, dispersing for 0.5h by ultrasonic, introducing nitrogen at room temperature for protection, adding 0.45g of potassium persulfate, reacting for 1h, heating to 65 ℃ for continuous reaction for 2h, alternately washing with absolute ethyl alcohol and water for 3 times, and drying in a vacuum box at 60 ℃ for 3h to obtain modified TiO 2
Step two: modified TiO 0.6g 2 Adding the mixture into 50mL of deionized water, magnetically stirring the mixture for 2 hours, and performing ultrasonic treatment for 2 hours to obtain modified TiO 2 Sol;
step three: adding 8g of flax fiber and 2g of rosin into a double-screw extruder, uniformly mixing, extruding composite master batch, putting into a drying oven for drying, adding into a spinning machine for melt blowing, drafting, degassing and drying, and collecting to obtain primary composite fiber;
step four: immersing 1g of the primary composite fiber obtained in the second step into 1.3g of modified TiO obtained in the first step 2 Sol and 0.15g of pentaneAnd (3) adhering the fibers in dialdehyde, uniformly stirring, and carrying out coagulating bath, ethanol washing and water washing, and airing to constant weight to obtain the self-cleaning textile fiber.
Example 3
The preparation process of the self-cleaning textile fiber comprises the following specific steps:
step one: first 2.3g oleic acid and 2.5g TiO were added 2 Adding (50 nm) into 50mL of dimethylbenzene, stirring for 3h, centrifugally filtering, washing with ethanol solution for 3 times, drying at 60 ℃, grinding, and sieving with a 300-mesh sieve to obtain stearic acid grafted TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the 2g of stearic acid is grafted with TiO 2 Adding 3g of 4-vinylbenzoic acid and 1g of 4-vinylaniline into 400mL of deionized water, dispersing for 0.5h by ultrasonic, introducing nitrogen at room temperature for protection, adding 0.45g of ammonium persulfate, reacting for 1h, heating to 65 ℃ for continuous reaction for 2h, alternately washing with absolute ethyl alcohol and water for 3 times, and drying in a vacuum box at 60 ℃ for 3h to obtain modified TiO 2
Step two: adding modified TiO2 of which the weight is 0.6g into 50mL of deionized water, magnetically stirring for 2 hours, and performing ultrasonic treatment for 2 hours to obtain modified TiO 2 Sol;
step three: adding 7g of regenerated cellulose fibers and 2g of rosin into a double-screw extruder, uniformly mixing, extruding composite master batch, drying in an oven, adding into a spinning machine for melt blowing, drafting, degassing and drying, and collecting to obtain primary composite fibers;
step four: immersing 1g of the primary composite fiber obtained in the second step into 1.4g of modified TiO obtained in the first step 2 The sol and 0.2g of succinic acid are adhered, stirred uniformly, and dried to constant weight through coagulating bath, ethanol washing and water washing to obtain the self-cleaning textile fiber.
Comparative example 1
Step one: will be 0.6g TiO 2 (50 nm) is added into 50mL of deionized water, and after magnetic stirring for 2h, ultrasonic treatment is carried out for 2h, thus obtaining modified TiO 2 Sol;
step two: adding cotton fiber and rosin into a double-screw extruder, uniformly mixing, extruding composite master batch, putting into a drying oven for drying, adding into a spinning machine for melt blowing, drafting, degassing and drying, and collecting to obtain primary composite fiber;
step three: immersing the primary composite fiber obtained in the second step into the modified TiO obtained in the first step 2 The sol and butane tetracarboxylic acid are adhered, stirred uniformly, and dried to constant weight through coagulating bath, ethanol washing and water washing to obtain the self-cleaning textile fiber.
Comparative example 2
The only difference from example 2 is that:
step three: adding flax fibers into a double-screw extruder, uniformly mixing, extruding composite master batch, drying in an oven, adding into a spinning machine for melt blowing, drafting, degassing and drying, and collecting to obtain the primary composite fibers.
Comparative example 3
The only difference from example 3 is that:
step four: immersing the primary composite fiber obtained in the second step into the modified TiO obtained in the first step 2 And (3) adhering the fibers in the sol, uniformly stirring, and carrying out coagulating bath, ethanol washing and water washing, and airing to constant weight to obtain the self-cleaning textile fibers.
Tests were performed on examples 4-6 and comparative examples 1-3:
the surface morphology of the fibers was observed using a scanning electron microscope (Regulus 8100), and the average diameter of 100 fibers was analyzed using Image J software.
Hydrophobic test: the fibers were adhered to a glass slide, and a 5. Mu.l drop was removed by a microsyringe to conduct a test, and the contact angle of the fibers was measured using a contact angle meter (JC 2000C 1).
And (3) self-cleaning effect test: sticking the fiber on a glass slide, then placing the glass slide on a glass dish, enabling the inclination angle of the glass slide and a horizontal table top to be 20 degrees, weighing rhodamine B dye with equal mass to be placed on the surface of the fiber, dripping deionized water with equal mass on the fiber, and observing the self-cleaning effect: the rhodamine B dye is simulated to be a 'stain', all or part of red marks are observed, the 'stain' is not self-cleaned or is not completely self-cleaned, no red marks are observed, the 'stain' is completely taken away by liquid drops, and the self-cleaning is completed.
The results are shown in Table 1:
TABLE 1
As can be seen from table 1, examples 1 to 3 have excellent hydrophobic effect and self-cleaning effect compared to comparative examples 1 to 3.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
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.

Claims (8)

1. The preparation process of the self-cleaning textile fiber is characterized by comprising the following steps of:
step one: stearic acid and TiO 2 Adding into dimethylbenzene, stirring, centrifugally filtering, washing, drying and grinding to obtain stearic acid grafted TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Grafting stearic acid to TiO 2 Adding 4-vinylbenzoic acid and 4-vinylaniline into deionized water, performing ultrasonic dispersion, introducing nitrogen at room temperature for protection, adding an initiator for reaction, and heating to 65Reacting at-70 ℃, alternately washing with absolute ethyl alcohol and water, and vacuum drying to obtain modified TiO 2
Step two: modified TiO 2 Adding the mixture into deionized water, stirring and carrying out ultrasonic treatment to obtain modified TiO 2 Sol;
step three: the fiber and rosin are mixed according to the mass ratio of 7-10:1-2, adding the mixture into a double-screw extruder, uniformly mixing, extruding composite master batch, putting the mixture into a drying oven for drying, adding the mixture into a spinning machine for melt blowing, drafting, degassing and drying, and collecting the mixture to obtain primary composite fibers;
step four: immersing the primary composite fiber obtained in the second step into the modified TiO obtained in the first step 2 And (3) adhering the sol and the cross-linking agent, stirring, and carrying out coagulating bath, ethanol washing and water washing, and airing to constant weight to obtain the self-cleaning textile fiber.
2. The process for preparing a self-cleaning textile fiber according to claim 1, wherein the fiber comprises one of cotton fiber, flax fiber, regenerated cellulose fiber and bamboo charcoal fiber.
3. The process for preparing a self-cleaning textile fiber according to claim 1, wherein the stearic acid is one of oleic acid, tetradecanoic acid and n-heptanoic acid.
4. The process for preparing a self-cleaning textile fiber according to claim 1, wherein the initiator is one of potassium persulfate and ammonium persulfate.
5. The process for preparing a self-cleaning textile fiber according to claim 1, wherein the cross-linking agent is one of butane tetracarboxylic acid, glutaraldehyde and succinic acid.
6. The process for preparing self-cleaning textile fiber according to claim 1, wherein the stearic acid and TiO in the first step 2 And xylene in an amount ratio of 1.8 to 2.3g:2.2-2.5g:50mL; hardGrafting Ti O with fatty acid 2 The dosage ratio of 4-vinylbenzoic acid, 4-vinylaniline, deionized water and initiator is 2g:2-4g:1-2g:400mL:0.3-0.5g; in the second step, ti O is modified 2 And deionized water in the amount of 5-8g:500mL.
7. The process for preparing self-cleaning textile fiber according to claim 1, wherein the primary composite fiber and the modified TiO in the fourth step are 2 The mass ratio of the sol to the cross-linking agent is 1:1.2-1.5:0.1-0.2.
8. A self-cleaning textile fibre, characterized in that it is produced by the preparation process according to any one of claims 1-7.
CN202311731376.5A 2023-12-15 2023-12-15 Self-cleaning textile fiber and preparation process thereof Pending CN117626632A (en)

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Application Number Priority Date Filing Date Title
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