CN107385880B - Preparation method of high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber - Google Patents
Preparation method of high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber Download PDFInfo
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- CN107385880B CN107385880B CN201710725732.0A CN201710725732A CN107385880B CN 107385880 B CN107385880 B CN 107385880B CN 201710725732 A CN201710725732 A CN 201710725732A CN 107385880 B CN107385880 B CN 107385880B
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- 239000000835 fiber Substances 0.000 title claims abstract description 79
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 30
- 239000002245 particle Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000002657 fibrous material Substances 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 229920006052 Chinlon® Polymers 0.000 claims description 9
- 229920004933 Terylene® Polymers 0.000 claims description 9
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- ZICZZIRMOMXKDN-UHFFFAOYSA-N 2-[2-hydroxyethyl(octyl)amino]decan-1-ol Chemical compound C(CCCCCCC)C(N(CCO)CCCCCCCC)CO ZICZZIRMOMXKDN-UHFFFAOYSA-N 0.000 claims description 8
- 229920002972 Acrylic fiber Polymers 0.000 claims description 7
- 229920006231 aramid fiber Polymers 0.000 claims description 7
- 229940043237 diethanolamine Drugs 0.000 abstract description 7
- -1 dioctyl diethanol amine Chemical compound 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 21
- ZHIIUGIVMJPBFB-UHFFFAOYSA-N azane;ethene Chemical compound N.N.C=C ZHIIUGIVMJPBFB-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 230000032683 aging Effects 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- 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
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
-
- 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
- D06M2101/32—Polyesters
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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
-
- 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
- D06M2101/36—Aromatic polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Artificial Filaments (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber, which comprises the steps of pretreating the fiber by a sodium hydroxide solution, adding the pretreated fiber into a mixed solution of di (dioctyl diethanol amine pyrophosphoryl) ethylenediamine titanate, water and NaCl, carrying out hydrothermal reaction, adding the fiber subjected to the hydrothermal reaction into a mixed solution of ethanol, water and ammonia water, stirring, reacting, and drying the fiber to obtain the high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber. The product has simple preparation process, easily controlled conditions, simple preparation, convenient mass production and no pollution.
Description
Technical Field
The invention relates to a preparation method of composite fibers, in particular to a preparation method of high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fibers.
Background
With the improvement of living standard of people, the demand of multifunctional fiber materials is accelerated year by year, and the dosage is increased year by year. Therefore, the application space for developing the fiber material with the formaldehyde removing function is wide, the photocatalytic formaldehyde removing fiber has the advantages of mild reaction conditions, low energy consumption, less secondary pollution and the like, and becomes one of the main research directions of future formaldehyde removing fiber materials, and the photocatalytic formaldehyde removing fiber material with excellent performance requires high formaldehyde removing rate, good washing fastness, color fastness, luster and appearance to be basically unchanged, and simultaneously keeps the strength of the textile. Therefore, there are many technical problems to be solved in order to develop a good photocatalytic formaldehyde-removing fiber material.
In the actual process of doping the photocatalyst into fabric or coating textiles, the particle size of the particles is not easy to control, and the problems of uneven dispersion, particle agglomeration and the like can be caused; in addition, in the use process, due to strong oxidation-reduction property of photocatalysis, the fiber material or the adhesive for connecting the fiber material and the adhesive can be promoted to age prematurely; further, the photocatalytic activity is a material which exerts its effect by utilizing light energy, and when it is mixed into the interior of a fiber textile material, if the irradiation of sunlight is not sufficiently received, the photocatalytic activity is not exerted well. According to the invention, the rice-shaped titanium dioxide particles with higher crystallinity are grown on the fiber surface by an in-situ growth method, so that the composite fiber material with the formaldehyde removing function is prepared, and the method not only enhances the photocatalytic degradation effect of the composite fabric, but also enhances the connection fastness between the fibers and the titanium dioxide.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber, which has the technical characteristics of strong firmness, ageing resistance, high photocatalytic degradation efficiency, uniform particle dispersion, good adsorbability and the like.
In order to realize the purpose, the invention is realized by the following technical scheme:
a preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber comprises the following steps:
step 1): soaking 1.0-2.0 parts of fiber in 10-100 parts of sodium hydroxide solution with the concentration of 5.0-16mol/L for pretreatment for 10-30 minutes according to the parts by weight;
step 2): according to the mass portion, 1.0-5.0 portions of di (dioctyl diethanolamine pyrophosphoryl acid) ethanediammonium titanate with the concentration of 0.1-1.0mol/L and 10-100 portions of H2O, 1.0-20 parts of NaCl, and uniformly stirring to obtain a mixed solution A;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 5-10 hours at the temperature of 100-150 ℃;
step 4): according to the mass portion, 10-100 portions of ethanol and 10-50 portions of H2O, 1.0-10 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 5.0-20 hours;
step 6): placing the reacted fiber in the step 5) at 80-100 ℃, and drying for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Preferably, the fiber in the step 1) is one or two of terylene, aramid, acrylic fiber and chinlon.
The invention relates to a preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber, which comprises the following steps:
step 1): soaking 1.5 parts of fibers in 55 parts of sodium hydroxide solution with the concentration of 10.5mol/L for 20 minutes according to the parts by weight;
step 2): according to the mass portion, 3.0 portions of di (dioctyl diethanol amine pyrophosphoryl acid) ethylene diammonium titanate with the concentration of 0.55mol/L and 55 portions of H2O, 10.5 parts of NaCl, and uniformly stirring to obtain a mixed solution A;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 7.5 hours at 175 ℃;
step 4): according to the mass portion, 55 portions of ethanol and 30 portions of H2O, 5.5 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 12.5 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 90 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Preferably, the fiber in the step 1) is one or two of terylene, aramid, acrylic fiber and chinlon.
The invention has the beneficial effects that: 1) the prepared rice-grain-shaped titanium dioxide loaded composite fiber material with high crystallinity has regular appearance and uniform size of the titanium dioxide growing on the surface of the fiber; 2) the connection fastness between the titanium dioxide and the fiber is improved; 3) the product has simple preparation process, easily controlled conditions and convenient large-scale production; 4) the reaction condition is mild, the preparation is simple, the energy consumption is low, and the secondary pollution is less; 5) the particle size of the particles is easy to control, the particles are uniformly dispersed and are not easy to agglomerate; 6) ageing resistance and high photocatalytic degradation effect; 7) high formaldehyde adsorption capacity, good adsorption effect and long service life.
Drawings
FIG. 1 is a scanning electron micrograph of a composite fiber prepared according to the present invention;
FIG. 2 is a second scanning electron micrograph of the composite fiber prepared according to the present invention.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the embodiments of the present invention are not limited to the following examples.
Example 1 a method for preparing a formaldehyde-removing composite fiber loaded with highly crystalline rice-shaped titanium dioxide particles, comprising the steps of:
step 1): 1.0 part of fiber is placed in 10 parts of sodium hydroxide solution with the concentration of 5.0mol/L for soaking pretreatment for 10 minutes according to the parts by mass, wherein the fiber is any one or two of terylene, aramid fiber, acrylic fiber and chinlon;
step 2): according to the parts by mass, 1.0 part of di (dioctyl diethanol amine pyrophosphoryl acid group) ethylene diammonium titanate with the concentration of 0.1mol/L and 10 parts of H2O, 1.0 part of NaCl, and stirring uniformly to obtain a mixed solution A, wherein the bis (dioctyl diethanolamine pyrophosphoryl acid group) ethylene diammonium titanate enhances the mechanical properties such as tear strength, tensile strength and the like and aging resistance of the fiber;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 5 hours at the temperature of 100 ℃;
step 4): according to the mass portion, 10 portions of ethanol and 10 portions of H2O, 1.0 part of ammonia water is uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 5.0 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 80 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Example 2 a method for preparing a high-crystallinity rice-shaped titanium dioxide particle-supported formaldehyde-removing composite fiber, which comprises the following steps:
step 1): soaking 1.5 parts of fiber in 55 parts of sodium hydroxide solution with the concentration of 10.5mol/L for 20 minutes according to the parts by mass, wherein the fiber is any one or two of terylene, aramid fiber, acrylic fiber and chinlon;
step 2): according to the mass portion, 3.0 portions of di (dioctyl diethanol amine pyrophosphoryl acid) ethylene diammonium titanate with the concentration of 0.55mol/L and 55 portions of H2O, 10.5 parts of NaCl, and stirring uniformly to obtain a mixed solution A, wherein the bis (dioctyl diethanolamine pyrophosphoryl acid group) ethylene diammonium titanate enhances the mechanical properties such as tear strength, tensile strength and the like and aging resistance of the fiber;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 7.5 hours at the temperature of 125 ℃;
step 4): according to the mass portion, 55 portions of ethanol and 30 portions of H2O, 5.5 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 12.5 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 90 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Example 3 a method for preparing a high-crystallinity rice-shaped titanium dioxide particle-supported formaldehyde-removing composite fiber, comprising the following steps:
step 1): 2.0 parts of fiber is placed in 100 parts of sodium hydroxide solution with the concentration of 16mol/L for soaking pretreatment for 30 minutes according to the parts by mass, wherein the fiber is any one or two of terylene, aramid fiber, acrylon and chinlon;
step (ii) of2): according to the parts by mass, 5.0 parts of di (dioctyl diethanol amine pyrophosphoryl acid) ethylene diammonium titanate with the concentration of 1.0mol/L and 100 parts of H2O, 20 parts of NaCl are mixed and uniformly stirred to obtain a mixed solution A, and the mechanical properties such as tear strength, tensile strength and the like and aging resistance of the bis (dioctyl diethanolamine pyrophosphoryl acid) ethylene diammonium titanate reinforced fiber are improved;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 10 hours at the temperature of 150 ℃;
step 4): according to the mass portion, 100 portions of ethanol and 50 portions of H2O, uniformly mixing 10 parts of ammonia water to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 20 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 100 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Example 4 a method for preparing a high-crystallinity rice-shaped titanium dioxide particle-supported formaldehyde-removing composite fiber, comprising the steps of:
step 1): soaking 1.3 parts of fiber in 65 parts of 12mol/L sodium hydroxide solution for pretreatment for 22 minutes, wherein the fiber is one or two of terylene, aramid fiber, acrylic fiber and chinlon;
step 2): according to the parts by mass, 3.3 parts of di (dioctyl diethanol amine pyrophosphoryl acid) ethylene diammonium titanate with the concentration of 0.7mol/L and 60 parts of H2O, mixing 12 parts of NaCl, and uniformly stirring to obtain a mixed solution A, wherein the bis (dioctyl diethanolamine pyrophosphoryl acid group) ethylene diammonium titanate reinforced fiber has mechanical properties such as tear strength, tensile strength and aging resistance;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 8 hours at the temperature of 130 ℃;
step 4): according to the mass parts, 55 parts of BAlcohol, 35 parts of H2O, 6 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 13 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 95 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Example 5 a method for preparing a high-crystallinity rice-shaped titanium dioxide particle-supported formaldehyde-removing composite fiber, comprising the following steps:
step 1): 2.0 parts of fiber is placed in 50 parts of sodium hydroxide solution with the concentration of 12mol/L for soaking pretreatment for 18 minutes according to the parts by mass, wherein the fiber is any one or two of terylene, aramid fiber, acrylon and chinlon;
step 2): according to the mass portion, 3.5 portions of di (dioctyl diethanol amine pyrophosphoryl acid) ethylene diammonium titanate with the concentration of 0.65mol/L and 55 portions of H2O, 15 parts of NaCl are mixed and uniformly stirred to obtain a mixed solution A, and the mechanical properties such as tear strength, tensile strength and the like and aging resistance of the bis (dioctyl diethanolamine pyrophosphoryl) ethylene diammonium titanate reinforced fiber are improved;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 7 hours at the temperature of 150 ℃;
step 4): according to the mass portion, 55 portions of ethanol and 30 portions of H2O, 7 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 15 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 80 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (3)
1. A preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber is characterized by comprising the following steps:
step 1): soaking 1.5-2.0 parts of fiber in 55-100 parts of sodium hydroxide solution with the concentration of 10.5-16mol/L for pretreatment for 20-30 minutes according to the parts by weight; the fiber is any one or two of terylene, aramid fiber, acrylic fiber and chinlon;
step 2): according to the mass portion, 1.0-5.0 portions of di (dioctyl diethanolamine pyrophosphoryl acid) ethanediammonium titanate with the concentration of 0.1-1.0mol/L and 10-100 portions of H2O, 1.0-20 parts of NaCl, and uniformly stirring to obtain a mixed solution A;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 5-10 hours at the temperature of 100-150 ℃;
step 4): according to the mass portion, 10-100 portions of ethanol and 10-50 portions of H2O, 1.0-10 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 5.0-20 hours;
step 6): placing the reacted fiber in the step 5) at 80-100 ℃, and drying for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
2. A preparation method of a high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber is characterized by comprising the following steps:
step 1): soaking 1.5 parts of fibers in 55 parts of sodium hydroxide solution with the concentration of 10.5mol/L for 20 minutes according to the parts by weight;
step 2): according to the mass portion, 3.0 portions of concentrated solution are addedDi (dioctyl diethanolamine pyrophosphoryl) ethanediamine titanate with the degree of 0.55mol/L, 55 parts of H2O, 10.5 parts of NaCl, and uniformly stirring to obtain a mixed solution A;
step 3): adding the fibers pretreated in the step 1) into the mixed solution A, and carrying out hydrothermal reaction for 7.5 hours at the temperature of 125 ℃;
step 4): according to the mass portion, 55 portions of ethanol and 30 portions of H2O, 5.5 parts of ammonia water are uniformly mixed to obtain a mixed solution B;
step 5): placing the fiber subjected to the hydrothermal reaction in the step 3) into the mixed solution B, mixing and stirring at room temperature, and reacting for 12.5 hours;
step 6): and (3) drying the reacted fiber in the step 5) at 90 ℃ for a day and night to obtain the rice-shaped titanium dioxide loaded composite fiber material with high crystallinity.
3. The preparation method of the high-crystallinity rice-shaped titanium dioxide particle-loaded formaldehyde-removing composite fiber according to claim 2, wherein the preparation method comprises the following steps: the fiber in the step 1) is one or two of terylene, aramid fiber, acrylic fiber and chinlon.
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| CN103739011A (en) * | 2013-12-30 | 2014-04-23 | 中国科学院上海硅酸盐研究所 | Method for preparing three-dimensional multistage titanium dioxide slurry with micro-nano structure by one-pot method |
| CN104108752A (en) * | 2013-04-22 | 2014-10-22 | 南京大学扬州化学化工研究院 | Preparation method of titanium dioxide |
| CN105696308A (en) * | 2015-07-31 | 2016-06-22 | 四川大学 | Arranging method for loading nanometer titanium dioxide on textiles |
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| CN104108752A (en) * | 2013-04-22 | 2014-10-22 | 南京大学扬州化学化工研究院 | Preparation method of titanium dioxide |
| CN103739011A (en) * | 2013-12-30 | 2014-04-23 | 中国科学院上海硅酸盐研究所 | Method for preparing three-dimensional multistage titanium dioxide slurry with micro-nano structure by one-pot method |
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