CN107385880A - A kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre - Google Patents
A kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre Download PDFInfo
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- CN107385880A CN107385880A CN201710725732.0A CN201710725732A CN107385880A CN 107385880 A CN107385880 A CN 107385880A CN 201710725732 A CN201710725732 A CN 201710725732A CN 107385880 A CN107385880 A CN 107385880A
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- 239000000835 fiber Substances 0.000 title claims abstract description 86
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000002245 particle Substances 0.000 title claims abstract description 20
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- -1 ammonium titanate esters Chemical class 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000002657 fibrous material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 230000002378 acidificating effect Effects 0.000 claims abstract description 12
- 229940043237 diethanolamine Drugs 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 11
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 12
- 229920002972 Acrylic fiber Polymers 0.000 claims description 9
- 239000004952 Polyamide Substances 0.000 claims description 9
- 229920004933 Terylene® Polymers 0.000 claims description 9
- 229920006231 aramid fiber Polymers 0.000 claims description 9
- 229920002647 polyamide Polymers 0.000 claims description 9
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000004408 titanium dioxide Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000003712 anti-aging effect Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000012783 reinforcing fiber Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010063493 Premature ageing Diseases 0.000 description 1
- 208000032038 Premature aging Diseases 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Artificial Filaments (AREA)
Abstract
Disclosed by the invention is a kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre,Fiber is pre-processed through sodium hydroxide solution,It is added to the ammonium titanate esters of two (dioctyl diethanol amine pyrophosphoryl acidic group) second two,Water,In NaCl mixed solutions,Carry out hydro-thermal reaction,Fiber Jing Guo hydro-thermal reaction is added to ethanol,Water,Stirred in ammoniacal liquor mixed solution,Reaction,Fiber is dried again,Obtain a kind of high-crystallinity rice-shaped TiO 2 particles load removes formaldehyde composite fibre,The present invention prepares the rice-shaped titanium dichloride load complex fiber material of high-crystallinity,The titanium dioxide regular appearance of fiber surface growth,Size uniformity,Improve the connection fastness between titanium dioxide and fiber,The product preparation process is simple,Condition is easily controllable,Prepare simple,It is easy to large-scale production,Prepare pollution-free.
Description
Technical field
The present invention relates to a kind of preparation method of composite fibre, more specifically say, be related to a kind of high-crystallinity rice-shaped
TiO 2 particles load except the preparation method of formaldehyde composite fibre.
Background technology
As the improvement of people's living standards, the demand of multifunction fiber material is accelerated year by year, dosage improves year by year.Cause
This, the application space of fibrous material of the exploitation with function of removing formaldehyde will be very wide, and photocatalysis is except formaldehyde fibers are with its reaction bar
The advantages that part is gentle, energy consumption is low and secondary pollution is few, by as one of following main direction of studying for removing formaldehyde fibers material, property
Can excellent photocatalysis have except formaldehyde rate is high, washability is good, color fastness, gloss, outward appearance are basic except formaldehyde fibers material requirements
It is constant, while keep the strength of textile in itself.Therefore, there are problems to need to break through from technological layer, could develop
Go out good photocatalysis and remove formaldehyde fibers material.
During actual photochemical catalyst is to fabric incorporation or to fabric coating, its grain diameter is not easily controlled,
The problems such as having scattered uneven, particle agglomeration；In addition in use, due to the stronger oxidation-reduction quality of photocatalysis, meeting
Promote fibrous material in itself or be coupled both binder premature agings；Furthermore photocatalysis is played effectiveness using luminous energy
Material, when it is mixed into inside fiber textile material, if can not fully receive the irradiation of sunshine, it cannot also send out well
Wave photocatalysis.The present invention grows the higher rice-shaped titanium dioxide of crystallinity by situ synthesis on the fiber surface
Particle, prepares the complex fiber material with function of removing formaldehyde, and this method not only increases the photocatalysis drop of composite material
Solve effect, while the connection fastness between reinforcing fiber and titanium dioxide.
The content of the invention
It is an object of the invention to solve problem of the prior art, there is provided have that firmness is strong, anti-aging, photocatalytic degradation
Efficiency high, particle are uniformly dispersed and a kind of load of high-crystallinity rice-shaped TiO 2 particles of the technical characterstic such as excellent adsorption
Except the preparation method of formaldehyde composite fibre.
To achieve the above object, the present invention is achieved by the following technical solutions：
A kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre, the preparation side
Method uses following steps：
Step 1)：By mass fraction, 1.0-2.0 part fibers are placed in the hydrogen-oxygen that 10-100 parts concentration is 5.0-16mol/L
Change dipping pretreatment 10-30 minutes in sodium solution；
Step 2)：By mass fraction, by two (dioctyl diethanol amine Jiao that 1.0-5.0 parts concentration is 0.1-1.0mol/L
Phosphinylidyne acidic group) two ammonium titanate esters of second, the H of 10-100 parts2The NaCl mixing of O, 1.0-20 part, stirs, obtains mixed solution
A；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 100-150 DEG C, water
Thermal response 5-10 hours；
Step 4)：By mass fraction, by the ethanol of 10-100 parts, the H of 10-50 parts2The ammoniacal liquor mixing of O, 1.0-10 part is equal
It is even, obtain mixed solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 5.0-20 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 80-100 DEG C, diel is dried, is obtained a kind of
The rice-shaped titanium dichloride load complex fiber material of high-crystallinity.
As a preferred embodiment, fiber described in step 1) is any one in terylene, aramid fiber, acrylic fibers and polyamide fibre or two
Kind.
A kind of present invention high-crystallinity rice-shaped TiO 2 particles load removes the preparation method of formaldehyde composite fibre, this
Preparation method uses following steps：
Step 1)：By mass fraction, 1.5 parts of fibers are placed in the sodium hydroxide solution that 55 parts of concentration are 10.5mol/L
Dipping pretreatment 20 minutes；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acid that 3.0 parts of concentration are 0.55mol/L
Base) two ammonium titanate esters of second, 55 parts of H2O, 10.5 parts of NaCl mixing, stirs, obtains mixed solution A；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 175 DEG C, hydro-thermal is anti-
Answer 7.5 hours；
Step 4)：By mass fraction, by 55 parts of ethanol, 30 parts of H2O, 5.5 parts of ammoniacal liquor are well mixed, mixed
Solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 12.5 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 90 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
As a preferred embodiment, fiber described in step 1) is any one in terylene, aramid fiber, acrylic fibers and polyamide fibre or two
Kind.
Beneficial effects of the present invention：1) the rice-shaped titanium dichloride load complex fiber material of high-crystallinity is prepared, it is fine
Tie up the titanium dioxide regular appearance of superficial growth, size uniformity；2) the connection fastness between titanium dioxide and fiber is improved；3)
The product preparation process is simple, and condition is easily controllable, is easy to large-scale production；4) reaction condition is gentle, it is simple to prepare, and energy consumption is low,
Secondary pollution is few；5) grain diameter is easy to control, is uniformly dispersed, and is not easy to reunite；6) anti-aging, photocatalytic degradation effect is high；7) inhale
Attached formaldehyde ability is high, advantages of good adsorption effect, service life length.
Brief description of the drawings
Fig. 1 is one of composite fibre stereoscan photograph prepared by the present invention；
Fig. 2 is the two of composite fibre stereoscan photograph prepared by the present invention.
Embodiment
Below by way of specific embodiment, the present invention is further illustrated, but embodiments of the present invention not by
The limitation of following examples.
A kind of load of the high-crystallinity rice-shaped TiO 2 particles of embodiment 1 except the preparation method of formaldehyde composite fibre,
The preparation method uses following steps：
Step 1)：By mass fraction, 1.0 parts of fibers are placed in the sodium hydroxide solution that 10 parts of concentration are 5.0mol/L and soaked
Bubble pretreatment 10 minutes, the fiber are any one or two kinds in terylene, aramid fiber, acrylic fibers and polyamide fibre；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acidic groups) that 1.0 parts of concentration are 0.1mol/L
The ammonium titanate esters of second two, 10 parts of H2O, 1.0 parts of NaCl mixing, stirs, obtains mixed solution A, the two (dioctyl two
Monoethanolamine pyrophosphoryl acidic group) mechanical performance such as two tearing toughness of ammonium titanate esters reinforcing fiber of second, tensile strength and anti-aging
Property；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 100 DEG C, hydro-thermal is anti-
Answer 5 hours；
Step 4)：By mass fraction, by 10 parts of ethanol, 10 parts of H2O, 1.0 parts of ammoniacal liquor are well mixed, mixed
Solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 5.0 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 80 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
A kind of load of the high-crystallinity rice-shaped TiO 2 particles of embodiment 2 except the preparation method of formaldehyde composite fibre,
The preparation method uses following steps：
Step 1)：By mass fraction, 1.5 parts of fibers are placed in the sodium hydroxide solution that 55 parts of concentration are 10.5mol/L
Dipping pretreatment 20 minutes, the fiber are any one or two kinds in terylene, aramid fiber, acrylic fibers and polyamide fibre；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acid that 3.0 parts of concentration are 0.55mol/L
Base) two ammonium titanate esters of second, 55 parts of H2O, 10.5 parts of NaCl mixing, stirs, obtains mixed solution A, described two (two is pungent
Base diethanol amine pyrophosphoryl acidic group) mechanical performance such as two tearing toughness of ammonium titanate esters reinforcing fiber of second, tensile strength and anti-
Aging；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 125 DEG C, hydro-thermal is anti-
Answer 7.5 hours；
Step 4)：By mass fraction, by 55 parts of ethanol, 30 parts of H2O, 5.5 parts of ammoniacal liquor are well mixed, mixed
Solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 12.5 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 90 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
A kind of load of the high-crystallinity rice-shaped TiO 2 particles of embodiment 3 except the preparation method of formaldehyde composite fibre,
The preparation method uses following steps：
Step 1)：By mass fraction, 2.0 parts of fibers are placed in the sodium hydroxide solution that 100 parts of concentration are 16mol/L and soaked
Bubble pretreatment 30 minutes, the fiber are any one or two kinds in terylene, aramid fiber, acrylic fibers and polyamide fibre；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acidic groups) that 5.0 parts of concentration are 1.0mol/L
The ammonium titanate esters of second two, 100 parts of H2O, 20 parts of NaCl mixing, stirs, obtains mixed solution A, the two (dioctyl two
Monoethanolamine pyrophosphoryl acidic group) mechanical performance such as two tearing toughness of ammonium titanate esters reinforcing fiber of second, tensile strength and anti-aging
Property；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 150 DEG C, hydro-thermal is anti-
Answer 10 hours；
Step 4)：By mass fraction, by 100 parts of ethanol, 50 parts of H2O, 10 parts of ammoniacal liquor are well mixed, mixed
Solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 20 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 100 DEG C, diel is dried, is obtained a kind of high
The rice-shaped titanium dichloride load complex fiber material of crystallinity.
A kind of load of the high-crystallinity rice-shaped TiO 2 particles of embodiment 4 except the preparation method of formaldehyde composite fibre,
The preparation method uses following steps：
Step 1)：By mass fraction, 1.3 parts of fibers are placed in the sodium hydroxide solution that 65 parts of concentration are 12mol/L and soaked
Bubble pretreatment 22 minutes, the fiber are any one or two kinds in terylene, aramid fiber, acrylic fibers and polyamide fibre；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acidic groups) that 3.3 parts of concentration are 0.7mol/L
The ammonium titanate esters of second two, 60 parts of H2O, 12 parts of NaCl mixing, stirs, obtains mixed solution A, the two (dioctyl two
Monoethanolamine pyrophosphoryl acidic group) mechanical performance such as two tearing toughness of ammonium titanate esters reinforcing fiber of second, tensile strength and anti-aging
Property；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 130 DEG C, hydro-thermal is anti-
Answer 8 hours；
Step 4)：By mass fraction, by 55 parts of ethanol, 35 parts of H2O, 6 parts of ammoniacal liquor are well mixed, and it is molten to obtain mixing
Liquid B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 13 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 95 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
A kind of load of the high-crystallinity rice-shaped TiO 2 particles of embodiment 5 except the preparation method of formaldehyde composite fibre,
The preparation method uses following steps：
Step 1)：By mass fraction, 2.0 parts of fibers are placed in the sodium hydroxide solution that 50 parts of concentration are 12mol/L and soaked
Bubble pretreatment 18 minutes, the fiber are any one or two kinds in terylene, aramid fiber, acrylic fibers and polyamide fibre；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryl acid that 3.5 parts of concentration are 0.65mol/L
Base) two ammonium titanate esters of second, 55 parts of H2O, 15 parts of NaCl mixing, stirs, obtains mixed solution A, the two (dioctyl
Diethanol amine pyrophosphoryl acidic group) mechanical performance such as two tearing toughness of ammonium titanate esters reinforcing fiber of second, tensile strength and anti-ageing
The property changed；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 150 DEG C, hydro-thermal is anti-
Answer 7 hours；
Step 4)：By mass fraction, by 55 parts of ethanol, 30 parts of H2O, 7 parts of ammoniacal liquor are well mixed, and it is molten to obtain mixing
Liquid B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mix at ambient temperature,
Stirring, react 15 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 80 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
Finally it should be noted that the invention is not restricted to above example, there can also be many variations.This area it is general
All deformations that logical technical staff directly can export or associate from present disclosure, it is considered as the present invention's
Protection domain.
Claims (4)
1. a kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre, it is characterised in that
The preparation method uses following steps：
Step 1)：By mass fraction, 1.0-2.0 part fibers are placed in the sodium hydroxide that 10-100 parts concentration is 5.0-16mol/L
Dipping pretreatment 10-30 minutes in solution；
Step 2)：By mass fraction, by two (the dioctyl diethanol amine pyrophosphoryls that 1.0-5.0 parts concentration is 0.1-1.0mol/L
Acidic group) two ammonium titanate esters of second, the H of 10-100 parts2The NaCl mixing of O, 1.0-20 part, stirs, obtains mixed solution A；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 100-150 DEG C, hydro-thermal is anti-
Answer 5-10 hours；
Step 4)：By mass fraction, by the ethanol of 10-100 parts, the H of 10-50 parts2The ammoniacal liquor of O, 1.0-10 part is well mixed, and is obtained
Obtain mixed solution B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mixes, stir at ambient temperature,
React 5.0-20 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 80-100 DEG C, diel is dried, obtains a kind of high knot
The rice-shaped titanium dichloride load complex fiber material of brilliant degree.
What 2. a kind of high-crystallinity rice-shaped TiO 2 particles according to claim 1 loaded removes formaldehyde composite fibre
Preparation method, it is characterised in that：Fiber described in step 1) is any one or two in terylene, aramid fiber, acrylic fibers and polyamide fibre
Kind.
3. a kind of load of high-crystallinity rice-shaped TiO 2 particles except the preparation method of formaldehyde composite fibre, it is characterised in that
The preparation method uses following steps：
Step 1)：By mass fraction, 1.5 parts of fibers are placed in the sodium hydroxide solution that 55 parts of concentration are 10.5mol/L and soaked
Pretreatment 20 minutes；
Step 2)：By mass fraction, by two (dioctyl diethanol amine pyrophosphoryl acidic group) second that 3.0 parts of concentration are 0.55mol/L
Two ammonium titanate esters, 55 parts of H2O, 10.5 parts of NaCl mixing, stirs, obtains mixed solution A；
Step 3)：Pretreated fiber in step 1) is added in mixed solution A, under the conditions of 125 DEG C, hydro-thermal reaction
7.5 hour；
Step 4)：By mass fraction, by 55 parts of ethanol, 30 parts of H2O, 5.5 parts of ammoniacal liquor are well mixed, and obtain mixed solution
B；
Step 5)：Fiber in step 3) Jing Guo hydro-thermal reaction is placed in mixed solution B, mixes, stir at ambient temperature,
Reaction 12.5 hours；
Step 6)：Under the conditions of fiber in step 5) by reaction is placed in into 90 DEG C, diel is dried, obtains a kind of high-crystallinity
Rice-shaped titanium dichloride load complex fiber material.
What 4. a kind of high-crystallinity rice-shaped TiO 2 particles according to claim 3 loaded removes formaldehyde composite fibre
Preparation method, it is characterised in that：Fiber described in step 1) is any one or two in terylene, aramid fiber, acrylic fibers and polyamide fibre
Kind.
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| CN112411177A (en) * | 2020-10-27 | 2021-02-26 | 深圳市铁汉人居环境科技有限公司 | Fiber comprising titanium dioxide nanostructure, preparation method and fabric |
| CN115247370A (en) * | 2021-11-12 | 2022-10-28 | 浙江理工大学 | Fiber material loaded with titanium dioxide particles and preparation method thereof |
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