CN110358329A - A kind of low cost Fypro titanium dioxide delustering agent and its preparation and application - Google Patents
A kind of low cost Fypro titanium dioxide delustering agent and its preparation and application Download PDFInfo
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- CN110358329A CN110358329A CN201910573992.XA CN201910573992A CN110358329A CN 110358329 A CN110358329 A CN 110358329A CN 201910573992 A CN201910573992 A CN 201910573992A CN 110358329 A CN110358329 A CN 110358329A
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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Abstract
The present invention relates to a kind of inexpensive Fypro titanium dioxide delustering agent and its preparations and application.The delustering agent includes stratum nucleare anatase phase titanium dioxide, is successively coated on the unformed silicon clad, unformed aluminium clad and outermost anionic surfactant modified layer on stratum nucleare anatase phase titanium dioxide surface.The preparation method includes: to be sequentially prepared unformed silicon clad, unformed aluminium clad on anatase titanium white superfine powder surface, is then carried out by anionic surfactant organically-modified.The utilization rate of expensive aluminium modifying agent is improved 12.9% by preparing unformed silicon clad by this method；By preparing aluminium clad, the grafting rate of anionic surfactant is improved 3 times；This method reaction condition is mild, is suitble to scale and serialization industrial production, significantly reduces process costs.
Description
Technical field
The invention belongs to delustering agent and its preparation and application field, in particular to a kind of inexpensive Fypro titanium white
Powder delustering agent and its preparation method and application.
Background technique
Fypro is commonly called as nylon or polyamide fibre, has good comprehensive performance, as light, hydrophilic, mechanical property is good, resistance to
Hot, wear-resistant and chemical-resistant resistance etc..Nylon fibre fabric has good intensity height, resilience, endurance, stainability good and resistance to
The resistance to equal excellent performances of damaging by worms of burn into.Nylon fibre product is in fields such as military-civil clothes, footgear, swimming suit, carpet decorations by wide
Big consumer's likes.However, have greatly light nylon fibre gloss it is dazzling, without pendency sense and it is transparent.In order to solve these problems, may be used
Fibre composition is improved, is usually added in synthetic fibers a certain amount of with biggish with fibre-forming polymer refractive index
Functional inorganic powder is prepared into semi-dull or full-dull product.
Anatase titanium dioxide is high with whiteness, refractive index is high, larger with fibre-forming polymer refractive index, nontoxic,
The advantages that low production cost and extensive raw material sources, is answered in the production of delustring nylon fibre as delustering agent extensively
With.However, titanium dioxide used in the industry giant of polyamide fibre is purchased from the Sha Haliben of Germany at present, international titanium dioxide in recent years
Price sharp rises, limits to plus manufacturer's production capacity, and the price of full-dull nylon fiber has not only been raised using import titanium dioxide,
The production capacity expansion of associated companies is constrained, so the delustering agent of developing low-cost has become numerous domestic titanium dioxide manufacturer and brocade
The research direction of synthetic fibre leading enterprise.
Even import titanium dioxide, partial size is not able to satisfy the requirement of best extinction effect still, and (partial size should meet visible light
The half of wavelength).Also, titanium white superfine powder large specific surface area, surface can be high, are also easy to produce reunion.Since addition titanium dioxide can only
Selection is added to the polymerization of nylon monomer, has high requirement to the particle size of titanium dioxide, distribution and bulky grain accounting,
These parameters directly affect the working life of filament spinning component and finally influence the performance and price of product.In addition, anatase titanium
White powder photocatalytic activity with higher itself totally disappeared fiber optics after by long-time illumination, easily lead to macromolecular chain in polymer
Fracture, polyamides amine degradation, polyamide fibre aging xanthochromia, mechanical properties decrease.At the same time, the photocatalysis of titanium dioxide can decompose fibre
The dye molecule for tieing up dyeing causes the weatherability of fiber and dyefastness to be deteriorated, so need to carry out titanium dioxide surface respectively
The finishing of multiple processes such as inorganic coating, organic coated is handled, to develop delustring Fypro with high performance titanium dioxide.
The technical study of current inorganic alclad is more, but aluminium coating agent easily crystallizes, and generates into nuclear envelope, is unfavorable for reducing titanium
The photocatalytic activity of white powder, and the conversion ratio of aluminium is lower, leads to increased costs；In organically-modified, silane coupling agent, titanate esters are even
It is relatively broad to join the use such as agent, but its effective grafting rate is for up to 20%, conversion ratio is extremely low, is unfavorable for the principle of low cost.
The patent of publication number CN103333527A discloses a kind of manufacturing method of polyamide fibre chemical fibre surface dulling agent.Specifically
Disclose during inorganic coating with silicon alkoxide, Titanium alkoxides or both mixture, titanium dioxide surface coat one layer it is amorphous
Silicon or titanium, increase the weatherability of titanium dioxide, but using silicon as inorganic coating layer, and it is poor to easily lead to Titanium dioxide slurry strainability,
Spinning plate is easily blocked in spinning process, not only will affect the service life of filament spinning component, also will affect the spinnability of nylon fibre；
Compounding side's coupling agent containing amino and epoxy group is used in organic graft modification, improves the dispersion stabilization of titanium dioxide, but its
Organically-modified using " one kettle way " progress, the grafting conversion ratio for easily leading to modifying agent reduces, and causes the increase of production cost.Due to
Cation modifier is expensive and toxic, uses anionic surfactant, but such coating titanium dioxide in industry mostly
Surface is negative potential, is unfavorable for improving anion-modified dose of service efficiency, increases cost.
The patent of publication number CN107541097A discloses a kind of preparation method of inorganic and organic coated titanium dioxide.Tool
Body is disclosed using NaAlO2Solution prepares alclad titanium dioxide, recycles Methyl Hydrogen Polysiloxane Fluid and hexamethyldisilazane to alclad
Titanium dioxide progress is organically-modified, solves pollution problem of the existing titanium dioxide organic agent to environment.But it is such directly to add
The method for coating for entering inorganic aluminate, causes the concentration of aluminium salt in system higher, occupies main advantage at nuclear envelope, causes aluminium salt sharp
It is low with rate, and the titanium dioxide of such organically-modified method preparation generates hydrophobic polymeric and due to modified production easily in caprolactam
Raw higher surface tension will lead to itself and Fypro poor compatibility, be unfavorable for the promotion of nylon fibre mechanical property, with
This simultaneously, compared with anionic surfactant, above two organic modifiers are expensive, be unfavorable for industrialization it is practical need
It asks.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of inexpensive Fypro titanium dioxide delustering agent and its
Preparation and application, with overcome in the prior art delustering agent lead to that Fypro poor mechanical property, dispersion stabilization be poor, extinction
Can be bad the defects of.
The present invention provides a kind of Fypro titanium dioxide delustering agent, the delustering agent includes stratum nucleare Anatase two
Titanium oxide is successively coated on unformed silicon clad, the unformed aluminium clad on stratum nucleare anatase phase titanium dioxide surface, and
Outermost anionic surfactant modified layer.
The anionic surfactant is neopelex, in lauryl sodium sulfate, sodium secondary alkyl sulfonate
One or two.
The present invention also provides a kind of Fypro preparation methods of titanium dioxide delustering agent, comprising:
It is sequentially prepared unformed silicon clad, unformed aluminium clad on anatase titanium white superfine powder surface, is then passed through
Anionic surfactant progress is organically-modified, obtains Fypro titanium dioxide delustering agent, wherein anion surface active
The mass ratio of agent and anatase titanium white superfine powder is 1~5:100.
The partial size of the anatase titanium white superfine powder is 0.2~0.4 μm.
The preparation method of the anatase titanium white superfine powder includes: to disperse anatase titanium dioxide in deionized water, is added
Enter dispersing agent and be uniformly mixing to obtain the titanium dioxide crude product slurry that concentration is 20~40wt%, grinding is washed to get wherein dispersing
Agent quality is 0.3~0.5wt% of anatase titanium dioxide quality.
The dispersing agent is at least one of calgon, polyethylene glycol, caprolactam.
The grinding is using grinder, and grinder rotating speed is 2000~2500r/min, and milling time is 30~40min.
The method for being sequentially prepared unformed silicon clad, unformed aluminium clad on anatase titanium white superfine powder surface
Include: that the stirring of anatase titanium white micropowder slurry, ultrasound are prepared into pre-dispersed slurry, silicon source precursor solution is added, maintains body
Be pH be 8.5~10.5, ageing adds silicon source precursor solution, and maintenance system pH is 7.5~9.5, ageing to get, wherein
Silicon source presoma is with SiO2Meter is 0.5~1.5:100 with the mass ratio of anatase titanium white superfine powder, silicon source presoma with
Al2O3Meter, the mass ratio with superfine powder are 2~4:100.
The ultrasonic time is 20~30min.
The speed of agitator is 300~500r/min.
The drop rate of the silicon source precursor solution is 80~100ml/ (hmol).
The drop rate of source of aluminium precursor solution is 80~100ml/ (hmol).
The addition silicon source precursor solution with silicon source precursor solution is added is carried out under 60~80 DEG C of heating.
The Aging Temperature is 60~80 DEG C, and digestion time is 1.5~2h.
The silicon source presoma is sodium metasilicate or nine water sodium metasilicate；Silicon source precursor solution concentration is 0.2~0.4mol/L.
Source of aluminium presoma is sodium metaaluminate；Silicon source precursor solution concentration is 0.5~0.6mol/L.
It is described that organically-modified method is carried out by anionic surfactant includes: by anionic surfactant-second
Alcoholic solution is added in sial coating Titanium dioxide slurry, and being modified makes long chain anionic group successfully graft on amorphous silicon aluminium packet
The surface of film titanium dioxide, gained is pulp centrifuged, washing, dry, crushing.
The anionic surfactant is neopelex, in lauryl sodium sulfate, sodium secondary alkyl sulfonate
One or two.
The modification temperature is 60~80 DEG C, and modification time is 3~4h.
The time for adding of the anionic surfactant-ethanol solution is 30~60min.
The stirring rate of the modification is 300~500r/min.
The washing uses ethanol washing 3~5 times；Drying time is 12h, and drying temperature is 80 DEG C.
The present invention also provides a kind of applications of above-mentioned delustering agent.
The present invention utilizes acid-base neutralization coprecipitation, in conjunction with sial bilayer envelope design, is changed by regulation pH value to adjust
Property agent hydrolysis reaction rate, make hydrolysate in mixed liquor with TiO2For core base, it is uniformly slowly coated on titanium dioxide
Surface forms fine and close amorphous clad, can effectively close the photocatalytic activity site on titanium dioxide surface, reduces photocatalysis
Activity, while silicon clad increases titanium dioxide surface negative potential, improves the transformation efficiency of aluminium modifying agent, has saved cost.
Furthermore the problem of slurry transmitance difference when the present invention also can be relieved single packet silicon using fine and close outermost aluminium clad, also can be changed titanium
The characteristics of surface electrical behavior of white powder turns negative number to positive number is carried out organic graft modification, is not only increased using anionic surfactant
The transformation efficiency of organic modifiers also helps the dispersion stabilization for keeping titanium dioxide delustering agent in polymerization spinning process, institute
It is as shown in Figure 1 to obtain product structure schematic diagram.
Beneficial effect
(1) preparation process of the present invention is simple, and reaction condition is mild, is suitble to industrial scale production, passes through sial coating
Double layer design not only improves the problem of single silicon coating transmitance difference, also solves the disadvantage that single aluminium coating easily crystallizes, and simultaneously will
The utilization rate of expensive aluminium covering improves 12.9%.
(2) present invention forms core-shell structure, i.e., in the amorphous silicon aluminium layer of the surface coated densification of anatase titania
The photocatalytic activity of titanium dioxide is inhibited, and the surface potential of titanium dioxide is positive by negative transformation, is conducive to cheap, nontoxic
Harmless anionic surfactant it is organically-modified, its utilization rate is improved 3 times, has saved cost.
(3) the long chain anionic bioactive molecule that is grafted of the present invention improves the compatible of delustering agent powder and Fypro
Property, increases intergranular steric hindrance, is conducive to delustering agent powder being uniformly distributed in the fibre, not only increases fiber
Elongation at break also greatly improves the ultraviolet-resistent property of fabric.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the modified titanium dioxide of the present invention；
Fig. 2 is the grading curve figure of anatase titanium white superfine powder grinding front and back prepared by embodiment 1；
Fig. 3 is the TEM photo of sial coating titanium dioxide prepared by embodiment 1；
Fig. 4 is the O 1s swarming figure of sial cladding front and back titanium dioxide XPS in embodiment 1；
Fig. 5 is sial cladding front and back titanium dioxide Zeta potential figure in embodiment 1；
Fig. 6 is that sial coats front and back titanium ore titanium dioxide to the degradation curve figure of azophloxine photoinitiator dye in embodiment 1；
Fig. 7 is the conversion ratio figure of sial coating titanium dioxide aluminium modifying agent prepared by embodiment 2；
Fig. 8 is the infrared figure of rear sial coating titanium dioxide Fourier before modified prepared by embodiment 2；
Fig. 9 be the sial coating titanium dioxide anionic surfactant for preparing of embodiment 2 before modified after and pure titanium dioxide
Anionic surfactant before modified after thermogravimetric curve figure；
It is complete that Figure 10 is that the surfactant-modified front and back sial coating titanium dioxide prepared using embodiment 2 is prepared as delustering agent
The stereoscan photograph of delustring polyamide slice profile；
It is complete that Figure 11 is that the surfactant-modified front and back sial coating titanium dioxide prepared using embodiment 2 is prepared as delustering agent
The stereoscan photograph of delustring Fypro section；
It is complete that Figure 12 is that the surfactant-modified front and back sial coating titanium dioxide prepared using embodiment 2 is prepared as delustering agent
The stereoscan photograph on delustring Fypro surface；
It is complete that Figure 13 is that the surfactant-modified front and back sial coating titanium dioxide prepared using embodiment 2 is prepared as delustering agent
Delustring Fypro Mechanics Performance Testing figure；
It is complete that Figure 14 is that the surfactant-modified front and back sial coating titanium dioxide prepared using embodiment 2 is prepared as delustering agent
Delustring polyamide fabric ultraviolet permeability figure；
Figure 15 is that surfactant-modified front and back sial coating titanium dioxide prepared by embodiment 2 makees delustering agent, preparation it is complete
Delustring polyamide fabric UV-vis DRS figure.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Anatase titanium dioxide is bought in Hebei Mai Sen titanium dioxide Co., Ltd, model NA100.
Embodiment 1
(1) it prepares anatase titanium white superfine powder: weighing 300g titanium dioxide crude product at room temperature and be dispersed in 450g deionized water,
1.50g calgon is added in magnetic agitation 5min, continues stirring 10min and obtains uniformly mixed Titanium dioxide slurry, then will
Slurry is slowly added into grinder, and the adjusting speed of mainshaft is 2500r/min, grinds 30min, is washed with spare.
Fig. 2 is the grading curve figure of grinding front and back anatase titanium dioxide, the results showed that the partial size of superfine powder after grinding
It is distributed in 0.2~0.4 μm and centralized particle diameter.
(2) sial coating titanium dioxide is prepared: by anatase titanium white micropowder slurry magnetic agitation obtained in step (1)
10min, ultrasonic disperse 20min；Then it places it in oil bath pan and is heated to 60 DEG C, stirring rate 300r/min, stir 15min
Afterwards, dropping evenly thereto by forming concentration with nine water sodium metasilicate of 4.73g and the configuration of 55.47mL deionized water is 0.3mol/L's
Solution, drop rate are then 90ml/ (hmol) is aged 1.5h, is obtained silicon with 1.6wt% sulfuric acid adjustment and control system pH=9.5
Coat Titanium dioxide slurry；Stated in slurry then up drop evenly by 4.82g sodium metaaluminate and 98.0mL deionized water configuration and
The solution for being 0.6mol/L at concentration, drop rate is 80ml/ (hmol), with 1.6wt% sulfuric acid adjustment and control system pH=8.5,
Then it is aged 1.5h, obtains sial cladding Titanium dioxide slurry.
Fig. 3 is the TEM figure of titanium dioxide after amorphous silicon aluminium cladding, it is known that titanium dioxide surface forms one layer of unbodied shell
Structure, coating is fine and close, film layer is continuous whole.
Fig. 4 is the XPS O 1s swarming figure that sial coats front and back titanium dioxide, it is known that clad part is in a manner of chemical bond
Connect with base nuclear phase.
Fig. 5 is titanium dioxide Zeta potential figure before and after sial coating, and titanium dioxide negative potential increases after silicon coats, outermost layer aluminium
Titanium dioxide surface potential is by the negative raising for switching to just be conducive to aluminium covering Yu anionic surfactant conversion ratio after cladding.
Fig. 6 is that cladding front and back anatase titanium dioxide light degradation azophloxine dyestuff degradation efficiency changes with light application time
Curve graph, sial coating titanium dioxide only has the 1/4 of non-coating to the degradation rate of simulation dye molecule after illumination 120min.
(3) it anionic surfactant method graft modification: by 1.0g sodium secondary alkyl sulfonate, is dissolved in 30mL dehydrated alcohol, obtains
To mixed solution and drop evenly in the cladding Titanium dioxide slurry of sial obtained by step (2), time for adding 30min, at 60 DEG C
Oil bath heating, while the rate magnetic agitation of 300r/min and to be condensed back, then modification time 3h is naturally cooled to
Room temperature with ethanol washing 3 times and is centrifuged, the last dry 12h in 80 DEG C of baking oven, crushes, obtain Fypro titanium white
Powder delustering agent.
Embodiment 2
(1) it prepares anatase titanium white superfine powder: weighing 300g titanium dioxide crude product at room temperature and be dispersed in 1200g deionized water
In, 0.90g polyethylene glycol is added in magnetic agitation 5min, continues stirring 10min and obtains uniformly mixed Titanium dioxide slurry, then
Slurry is slowly added into grinder, the adjusting speed of mainshaft is 2000r/min, grinds 40min, is washed with spare.
(2) sial coating titanium dioxide is prepared: by anatase titanium white micropowder slurry magnetic agitation obtained in step (1)
10min, ultrasonic disperse 30min；Then it places it in oil bath pan and is heated to 80 DEG C, stirring rate 500r/min, stir 15min
Afterwards, dropping evenly thereto by forming concentration with nine water sodium metasilicate of 7.10g and the configuration of 62.4mL deionized water is 0.4mol/L's
Solution, drop rate are then 80ml/ (hmol) is aged 2.0h, is obtained silicon with 1.6wt% sulfuric acid adjustment and control system pH=8.5
Coat Titanium dioxide slurry；It states in slurry and is dropped evenly by being configured with 6.43g sodium metaaluminate and 117.6mL deionized water then up
The solution for being 0.5mol/L into concentration, drop rate is 100ml/ (hmol), with 1.6wt% sulfuric acid adjustment and control system pH=
7.5, it is then aged 2.0h, obtains sial cladding Titanium dioxide slurry.
(3) anionic surfactant method graft modification: by 5.0g neopelex, it is dissolved in the anhydrous second of 60mL
Alcohol obtains mixed solution and drops evenly in the cladding Titanium dioxide slurry of sial obtained by step (2), time for adding 60min, 80
Oil bath heating at DEG C, while the rate magnetic agitation of 500r/min and to be condensed back, modification time 4h is then naturally cold
But it to room temperature, with ethanol washing 3 times and is centrifuged, the last dry 12h in 80 DEG C of baking oven, crushes, obtain Fypro use
Titanium dioxide delustering agent.
Full-dull polyamide slice the preparation method comprises the following steps: weigh 2.0kg caprolactam heating melting, 40.0g 12 is added
The modified sial of sodium alkyl benzene sulfonate coats titanium dioxide, is added in 5L polymeric kettle after emulsion dispersion, nitrogen is passed through into polymeric kettle
Gas is slowly warming up to 255 DEG C to exclude air, and pressure is kept to lay down after 0.6~0.7MPa, stirring rate 200r/min, 3h
Pressure and it is continually fed into nitrogen in kettle, after electric current is stablized, the reaction was continued 1h finally squeezes into nitrogen discharging, pelletizing, totally disappeared
Light polyamide slice.It is to have light polyamide to cut greatly that delustering agent titanium dioxide, which is not added with, by the slice of polyamide prepared by above-mentioned technique
Piece.
Feed inlet is added the preparation method comprises the following steps: full-dull polyamide is sliced in full-dull Fypro, melts at 270 DEG C
It is extruded after melting through spinneret orifice, spinneret hole count is 36, component pressure 50kg, then oils, is pre-stretched, winds, finally with leading in parallel
The drawing-off that machine carries out certain 3.4 multiple is stretched, draft speed 250m/min obtains full-dull Fypro.There to be light polyamides greatly
Amine slice is to have light Fypro greatly according to fiber prepared by above-mentioned preparation process.
Full-dull polyamide fabric the preparation method comprises the following steps: by full-dull Fypro use longitude and latitude weaving, through adding
Twirl thermal finalization, heald, denting, warping prepare full-dull polyamide fabric.There to be light Fypro according to above-mentioned volume greatly
Weaving process fabric obtained is to have light polyamide fabric greatly.
Fig. 7 is the conversion ratio figure of sial coating titanium dioxide aluminium modifying agent, as seen from the figure, the conversion ratio of aluminium modifying agent after packet silicon
Improve 12.9%.
Fig. 8 be neopelex before modified after sial coating titanium dioxide the infrared figure of Fourier, it is modified sharp
Titanium ore titanium dioxide is respectively in 2960.4cm-1、2896.8cm-1、885.1cm-1There is-CH respectively in place2Flexible and bending vibration
The absorption peak of absorption peak, phenyl ring can belong to-CH in modifying agent neopelex2With the presence of benzene radicals, explanation
Its surface is successfully grafted long-chain molecule.
Fig. 9 is neopelex rear sial coating titanium dioxide or pure titanium dioxide thermogravimetric curve figure before modified, by
Long-chain molecule grafting amount improves 3 times than non-coating grafting rate up to 2.72% known to figure.(wherein neopelex
In addition to not having to carry out sial cladding, other are identical as above-mentioned delustering agent for the preparation of pure titanium dioxide after before modified)
Figure 10 be the neopelex that prepare using embodiment 2 before modified afterwards sial coating titanium dioxide as delustering agent system
Standby full-dull polyamide slice profile electromicroscopic photograph, wherein a figure is totally disappeared for not organically-modified sial cladding titanium dioxide preparation
The electromicroscopic photograph of light polyamide slice profile；B figure is through the modified sial cladding titanium dioxide preparation of neopelex
Full-dull polyamide slice profile electromicroscopic photograph.It can be seen from the figure that powder produces serious reunion, b figure in a figure
Middle titanium dioxide powder occurs and is evenly distributed without obvious reunion, illustrates through the modified sial cladding titanium of neopelex
The organic-chain molecules of white powder surface grafting had both produced the effect of steric hindrance, prevented the reunion of particle, also enhanced sial
Coat the compatibility of titanium dioxide and polyamide.
Figure 11 be the neopelex that prepare using embodiment 2 before modified afterwards sial coating titanium dioxide as delustering agent system
The stereoscan photograph of standby full-dull Fypro section, wherein a figure is not organically-modified sial cladding titanium dioxide preparation
Full-dull Fypro section electromicroscopic photograph；B figure is through the modified sial cladding titanium white of neopelex
The electromicroscopic photograph of the full-dull Fypro of powder preparation.It can be seen from the figure that powder produces sternly in fibrous inside in a figure
The reunion of weight, be because unmodified powder in inside produces hydrophobic polymeric, in b figure titanium dioxide powder without it is obvious reunite occur and
It is evenly distributed, illustrates to prevent through the organic-chain molecules of the modified sial cladding titanium dioxide surface grafting of neopelex
The reunion of particle.
Figure 12 is to coat the full-dull that titanium dioxide is prepared as delustering agent using the modified sial of neopelex to gather
The stereoscan photograph on nylon surface, wherein a figure is the full-dull polyamides of not organically-modified sial cladding titanium dioxide preparation
The electromicroscopic photograph of amine fiber surface；B figure is totally disappeared through the modified sial cladding titanium dioxide preparation of neopelex
The electromicroscopic photograph on light Fypro surface.It can be seen from the figure that powder in fiber surface has an aggregate appearance in a figure, b figure
Middle titanium dioxide powder is evenly distributed in fiber surface, is conducive to the extinction performance for improving fiber.
Figure 13 is that the full-dull prepared using the modified sial cladding titanium dioxide of neopelex as delustering agent gathers
The Mechanics Performance Testing figure of nylon, compared with having light Fypro greatly, due to the introducing of the organically-modified delustering agent of long-chain
It can be considered the physical crosslinking point inside full-dull Fypro, improve fiber creep-resistant property, increase its extension at break
Rate.
Figure 14 is that the full-dull prepared using the modified sial cladding titanium dioxide of neopelex as delustering agent gathers
The ultraviolet permeability figure of amide fabric, compared with having light polyamide fabric greatly, the decline of full-dull polyamide fabric ultraviolet permeability
12% or so, improve the uvioresistant performance of fabric.
Figure 15 is that the full-dull prepared using the modified sial cladding titanium dioxide of neopelex as delustering agent gathers
The UV-vis DRS figure of amide fabric, compared with having light polyamide fabric greatly, full-dull polyamide fabric is to visible light
Diffusing reflection improves 20% or so, effectively improves the extinction performance of fabric.
Embodiment 3
(1) it prepares anatase titanium white superfine powder: weighing 300g titanium dioxide crude product at room temperature and be dispersed in 700g deionized water,
1.20g caprolactam is added in magnetic agitation 5min, continues stirring 10min and obtains uniformly mixed Titanium dioxide slurry, then will slurry
Material is slowly added into grinder, and the adjusting speed of mainshaft is 2300r/min, grinds 35min, is washed with spare.
(2) sial coating titanium dioxide is prepared: by anatase titanium white micropowder slurry magnetic agitation obtained in step (1)
10min, ultrasonic disperse 25min；Then it places it in oil bath pan and is heated to 70 DEG C, stirring rate 400r/min, stir 15min
Afterwards, dropping evenly thereto by forming concentration with nine water sodium metasilicate of 2.37g and the configuration of 41.6mL deionized water is 0.2mol/L's
Solution, drop rate are then 100ml/ (hmol) is aged 1.5h, is obtained with 1.6wt% sulfuric acid adjustment and control system pH=10.5
Silicon coats Titanium dioxide slurry；It states in slurry and is dropped evenly by being matched with 3.22g sodium metaaluminate and 71.3mL deionized water then up
The solution for being 0.55mol/L into concentration is set, drop rate is 90ml/ (hmol), with 1.6wt% sulfuric acid adjustment and control system pH=
9.5, it is then aged 1.5h, obtains sial cladding Titanium dioxide slurry.
(3) anionic surfactant method graft modification: by 3.0g lauryl sodium sulfate, be dissolved in 45mL dehydrated alcohol,
It obtains mixed solution and drops evenly in the cladding Titanium dioxide slurry of sial obtained by step (2), time for adding 45min, at 70 DEG C
Lower oil bath heating, while the rate magnetic agitation of 400r/min and to be condensed back, modification time 3.5h is then naturally cold
But it to room temperature, with ethanol washing 3 times and is centrifuged, the last dry 12h in 80 DEG C of baking oven, crushes, obtain Fypro use
Titanium dioxide delustering agent.
103333527 A of Chinese patent CN discloses a kind of manufacturing method of the modified delustering agent in polyamide fibre chemical fibre surface, with
Anatase thpe white powder is raw material, deposits the amorphous titanium oxide that a layer thickness is 1-100nm on its surface by hydrolysis methods,
Then carried out with compounding side's coupling agent containing amino and epoxy group organically-modified, finally obtaining has in caprolactam-aqueous systems
The modified titanium of dispersibility and compatibility very well.
The present invention is compared with 103333527 A of Chinese patent CN, firstly, unformed packet in 103333527 A of patent CN
Coating raw material is Titanium alkoxides or silicon alkoxide, and price is costly compared to silicate and aluminate；Secondly of the invention unformed
Sial double layer design, the problem that the unformed aluminium clad of outer layer not only can solve silicon coating Titanium dioxide slurry transmitance difference can also change
The charge property (being changed into positive potential by negative potential under neutrallty condition) for becoming titanium dioxide surface, is conducive to nontoxic, at low cost
Honest and clean, raw material sources are extensive and the longer anionic surfactant graft modification of organic chain, in 103333527 A of patent CN
Compounding side's coupling agent it is expensive and be easy itself hydrolytic condensation, cause modifying agent utilization rate low, industrial cost increases.
Claims (10)
1. a kind of Fypro titanium dioxide delustering agent, which is characterized in that the delustering agent includes stratum nucleare Anatase dioxy
Change titanium, is successively coated on unformed silicon clad, the unformed aluminium clad on stratum nucleare anatase phase titanium dioxide surface, and most
The anionic surfactant modified layer of outer layer.
2. delustering agent according to claim 1, which is characterized in that the anionic surfactant is dodecyl benzene sulfonic acid
One or both of sodium, lauryl sodium sulfate, sodium secondary alkyl sulfonate.
3. a kind of Fypro preparation method of titanium dioxide delustering agent, comprising:
Be sequentially prepared unformed silicon clad, unformed aluminium clad on anatase titanium white superfine powder surface, then by yin from
Sub- surfactant carries out organically-modified, obtains Fypro titanium dioxide delustering agent, wherein anionic surfactant with
The mass ratio of anatase titanium white superfine powder is 1~5:100.
4. method according to claim 3, which is characterized in that the partial size of the anatase titanium white superfine powder is 0.2~0.4 μ
m；The preparation method of anatase titanium white superfine powder includes: to disperse anatase titanium dioxide in deionized water, and dispersing agent is added and stirs
The titanium dioxide crude product slurry for uniformly obtaining that concentration is 20~40wt% is mixed, grinding is washed to get wherein dispersing agent quality is sharp
0.3~0.5wt% of titanium ore titanium dioxide quality.
5. method according to claim 3, which is characterized in that described to be sequentially prepared on anatase titanium white superfine powder surface without fixed
Type silicon clad, unformed aluminium clad method include: by anatase titanium white micropowder slurry stirring, ultrasound prepare it is pre-dispersed
Silicon source precursor solution is added in slurry, and maintenance system pH is 8.5~10.5, and ageing adds silicon source precursor solution, maintains
System pH is 7.5~9.5, is aged to get wherein silicon source presoma is with SiO2Meter, the quality with anatase titanium white superfine powder
Than for 0.5~1.5:100, silicon source presoma is with Al2O3Meter, the mass ratio with superfine powder are 2~4:100.
6. method according to claim 5, which is characterized in that the addition silicon source precursor solution and add silicon source forerunner
Liquid solution is carried out under 60~80 DEG C of heating；Aging Temperature is 60~80 DEG C, and digestion time is 1.5~2h.
7. method according to claim 5, which is characterized in that the silicon source presoma is sodium metasilicate or nine water sodium metasilicate；Silicon
Source precursor solution concentration is 0.2~0.4mol/L；Silicon source presoma is sodium metaaluminate；Silicon source precursor solution concentration is 0.5
~0.6mol/L.
8. method according to claim 3, which is characterized in that it is described carried out by anionic surfactant it is organically-modified
Method includes: that anionic surfactant-ethanol solution is added in sial coating Titanium dioxide slurry, is modified, is centrifuged, washes
It washs, dry, crush.
9. method according to claim 8, which is characterized in that the anionic surfactant is dodecyl benzene sulfonic acid
One or both of sodium, lauryl sodium sulfate, sodium secondary alkyl sulfonate；Modification temperature be 60~80 DEG C, modification time be 3~
4h。
10. a kind of application of delustering agent as described in claim 1.
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