CN109837605A - Compound brush filament of a kind of titania modified polyester nano of two-dimensional ultrathin and preparation method thereof - Google Patents
Compound brush filament of a kind of titania modified polyester nano of two-dimensional ultrathin and preparation method thereof Download PDFInfo
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- CN109837605A CN109837605A CN201910089521.1A CN201910089521A CN109837605A CN 109837605 A CN109837605 A CN 109837605A CN 201910089521 A CN201910089521 A CN 201910089521A CN 109837605 A CN109837605 A CN 109837605A
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Abstract
The present invention provides compound brush filament of a kind of titania modified polyester nano of two-dimensional ultrathin and preparation method thereof, belongs to technical field of polymer materials.The compound brush filament is in parts by weight, composed of the following components: 60-96 parts of polyester, modified two-dimensional ultrathin nano-TiO20.1-20 parts, 0.5-2 parts of antioxidant, 0.5-8 parts of lubricant;The two-dimensional ultrathin nano-TiO of the modification2It is by two-dimensional ultrathin nano-TiO2Surfactant is added and carries out that surface is modified to be obtained;The two-dimensional ultrathin nano-TiO of the modification2It is less than 50nm for thickness, radius-thickness ratio is greater than 5.The present invention also provides a kind of preparation methods of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin.There is obvious concave-convex sense on polyester brush silk fiber surface of the invention, and performance and structure are similar to wool.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of titania modified polyester nano of two-dimensional ultrathin
Compound brush filament and preparation method thereof.
Background technique
Engineering plastics are widely used in fields such as electric appliance and electronic, automobile interior decoration, construction and decoration, Aerospace manufacturings, currently, in
State has become the most fast country of engineering plastics demand increase.Although polyester industrialization in polymer arts is later, by
It is with the fastest developing speed in five large-engineering plastics in its excellent performance.Polyester has excellent mechanical property, chemically-resistant rotten
Light up performance and good mobile performance, but polyester is crystallinity engineering plastics, shaping shrinkage rate is bigger than ingeniously, dimensional stability compared with
It is excessive to easily lead to product wing curvature in forming process for difference, to limit the application range of polyester article.In addition, exploitation one
The new high performance material difficulty of kind is larger, and the R&D cycle is long, expends fund and energy is big.Therefore, in order to meet not
Same purposes, optimal path are that polymer-filled is modified, by it is some from existing resin matrix in different inorganic of physicochemical properties
Filler, which is added in polymeric matrix, is modified research, and preparing one kind to it using chemical method or physical method has
The new composite of excellent performance.The advantages of this method is exactly succinct industrialized production effective, at low cost and easy, is greatly improved
The application value of polymer industrially.
Inorganic filler due to special physicochemical property, can significantly improve the mechanical property of polymer, forming property and
Hot property etc., therefore application development is rapid in polymer modification technology.
Summary of the invention
The purpose of the invention is to provide a kind of compound brush filament of the titania modified polyester nano of two-dimensional ultrathin and its system
Preparation Method.The compound brush filament of the polyester nano has good spinnability.
Present invention firstly provides a kind of two-dimensional ultrathin TiO2The nano combined brush filament of modified poly ester, in parts by weight, by
Following components composition:
60-96 parts of polyester, modified two-dimensional ultrathin nano-TiO20.1-20 parts, 0.5-2 parts of antioxidant, lubricant 0.5-8
Part;
The two-dimensional ultrathin nano-TiO of the modification2It is by two-dimensional ultrathin nano-TiO2Surfactant is added and carries out surface
It is modified to obtain;
The two-dimensional ultrathin nano-TiO of the modification2It is less than 50nm for thickness, radius-thickness ratio is greater than 5.
Preferably, the surfactant is one or both of KH550, KH560 or hexamethyldisilazane.
Preferably, the polyester is one of PET or PBT.
Preferably, the antioxidant is one or both of antioxidant 1010,1076, B900,3114.
Preferably, the lubricant is MoS2Or one or both of PETS-XY201A.
The present invention also provides a kind of preparation methods of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin, comprising:
Step 1: preparation two-dimensional ultrathin nano-TiO2
Under nitrogen protection, titanium tetrachloride is added into ethylene glycol, is heated to flowing back, water reaction is then added, obtains two
Tie up ultrathin nanometer TiO2;
Step 2: modified two-dimensional ultrathin nano-TiO2
By the two-dimensional ultrathin nano-TiO of surfactant and step 12Reaction, obtains modified two-dimensional ultrathin nano-TiO2;
Step 3: melt blending
By polyester, the two-dimensional ultrathin nano-TiO of modification2, antioxidant and lubricant be stirred and mix to uniform, obtain
Mixture is squeezed out by double screw extruder, is granulated, and pellet is obtained;
Step 4: spinning moulding
The pellet of step 3 is subjected to spinning moulding, obtains the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin.
Preferably, the volume ratio of ethylene glycol and titanium tetrachloride is (5-100) in the step 1: 1, titanium tetrachloride and water
Volume ratio be (1-4): 1.
Preferably, the reaction temperature of the step two is 60~80 DEG C, reaction time 2-6h.
Preferably, the extrusion temperature of the step 3 is 220-260 DEG C, screw speed 100-150r/min.
Preferably, the spinning moulding temperature of the step 4 is 220-260 DEG C.
Beneficial effects of the present invention
The present invention provides a kind of two-dimensional ultrathin TiO2Nano combined brush filament of modified poly ester and preparation method thereof, this method passes through
It joined the nano-TiO of modified two-dimensional ultrathin in polyester material2, by ultra-thin TiO2Nanometer sheet carries out surface and is modified, and uses
It fills polyester, so that it is uniformly dispersed in polyester matrix, and have good compatibility, so that polyester fiber has good spin
Property, the viscous powder amount of polyester brush filament is improved, quality is stablized, and fiber surface has obvious concave-convex sense, performance and structure and wool phase
Seemingly, added value of product is high, can be widely applied to all kinds of hairbrush of toothbrush, dust removal brush and cosmetic industry etc..
Detailed description of the invention
Fig. 1 is the surface sweeping electromicroscopic photograph that pure Direct-spinning of PET Fiber is 250 times in enlargement ratio.
Fig. 2 is the surface sweeping electromicroscopic photograph that pure Direct-spinning of PET Fiber is 1000 times in enlargement ratio.
Fig. 3 is the two-dimensional ultrathin nano-TiO that the embodiment of the present invention 2 is prepared2The nano combined spinning of modified poly ester is being put
The surface sweeping electromicroscopic photograph that big multiplying power is 650 times.
Fig. 4 is the two-dimensional ultrathin nano-TiO that the embodiment of the present invention 2 is prepared2The nano combined spinning of modified poly ester is being put
The surface sweeping electromicroscopic photograph that big multiplying power is 1000 times.
Specific embodiment
Present invention firstly provides a kind of compound brush filaments of the titania modified polyester nano of two-dimensional ultrathin, according to parts by weight
Meter, composed of the following components:
60-96 parts of polyester, modified two-dimensional ultrathin nano-TiO20.1-20 parts, 0.5-2 parts of antioxidant, lubricant 0.5-8
Part;It is preferred that are as follows: 92-96 parts of polyester, modified two-dimensional ultrathin nano-TiO20.5-4 parts, 1 part of antioxidant, 2.5-3 parts of lubricant;
The two-dimensional ultrathin nano-TiO of the modification2It is by two-dimensional ultrathin nano-TiO2Surfactant is added and carries out surface
It is modified to obtain;The surfactant is preferably one or both of KH550, KH560 or hexamethyldisilazane.
The present invention is by surfactant to two-dimensional ultrathin nano-TiO2It is modified to carry out surface, makes two-dimensional ultrathin nano-TiO2In polyester base
Dispersibility in body resin is more preferable, to improve the performance of polyester material.
The two-dimensional ultrathin nano-TiO of the modification2For thickness be less than 50nm, preferably 20, radius-thickness ratio be greater than 5, preferably
It is 10.The present invention limits the two-dimensional ultrathin nano-TiO of the modification2Thickness and radius-thickness ratio will affect polyester when thickness is excessively high
The spinning properties of fiber, thickness is bigger, and the spinnability of nanocomposite spinning is lower, when radius-thickness ratio is too small, will affect and receives
Dispersibility of the rice sheet layer material in polyester matrix, influences spinning effect, while also will affect the recessed of nano combined brush filament surface
Convex sense, lamella is too small, and the microstructure of imitative wool surfaces is not achieved in nano combined brush filament surface no concave-convex sense, causes nanometer multiple
The glutinous powder amount for closing brush filament can be greatly reduced.
According to the present invention, the polyester be preferably PET, PBT, one of, the antioxidant and lubricant are preferred
For the auxiliary agent of this field routine, the antioxidant is preferably one of antioxidant 1010,1076, B900,3114 or two
Kind;Lubricant is preferably MoS2Or one or both of PETS-XY201A.
The present invention also provides a kind of preparation methods of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin, comprising:
Step 1: preparation two-dimensional ultrathin nano-TiO2
Under nitrogen protection, titanium tetrachloride is added into ethylene glycol, is heated to flowing back, water reaction, reaction knot is then added
Shu Hou is cooled to room temperature, obtains two-dimensional ultrathin nano-TiO after centrifuge separation washing2;The reaction time is preferably 30min-
5h;The volume ratio of more preferably 2-4h, the ethylene glycol and titanium tetrachloride is preferably (5-100): 1, more preferably (5-6): 1,
The volume ratio of titanium tetrachloride and water is preferably (1-4): 1, more preferably (1-1.25): 1;The ethylene glycol is as directed agents;
Step 2: modified two-dimensional ultrathin nano-TiO2
By the two-dimensional ultrathin nano-TiO of surfactant and step 12Reaction, obtains modified two-dimensional ultrathin nano-TiO2;
It is particularly preferred as: by two-dimensional ultrathin nano-TiO2It is counter to be scattered in water and alcohol mixed solution, excusing from death dispersion, when the described dispersion
Between preferably 50-60min, then be added surfactant reaction, the reaction temperature is preferably 60~80 DEG C, and the time is preferred
For 2-6h, it is centrifuged after cooling, dry, the centrifugal rotational speed is preferably 4000-6000r/min, and drying temperature is preferably 60~
140 DEG C, drying time is preferably 12-24h;The additional amount of the surfactant is two-dimensional ultrathin nano-TiO2The 2- of quality
10%, more preferably 5%;
Step 3: melt blending
By polyester, the two-dimensional ultrathin nano-TiO of modification2, antioxidant and lubricant be stirred and mix to uniform, obtain
Mixture is squeezed out by double screw extruder, is granulated, and pellet is obtained;The two-dimensional ultrathin nano-TiO of the polyester, modification2Into
Before row mixing, preferably first it is dried respectively, to improve the processing performance of material, the drying temperature is preferably 95-125
DEG C, drying time is preferably 2-8 hours;The extrusion temperature is preferably 220-260 DEG C, and more preferably 230-240 DEG C, screw rod
Revolving speed is preferably 100-150r/min, more preferably 150r/min;
Step 4: spinning moulding
The pellet of step 3 is subjected to spinning moulding, the composite spun fiber that will be obtained after clipped is soaked in NaOH solution
Middle progress sharpening processing, obtains two-dimensional ultrathin TiO2The nano combined brush filament of modified poly ester.The spinning moulding temperature is preferably
220-260 DEG C, more preferably 230-235 DEG C;The concentration of the NaOH solution is preferably 30%.
Further detailed description is done to the present invention combined with specific embodiments below, the raw material being related in embodiment is
It is commercially available.
Embodiment 1
Under nitrogen protection, 0.5L titanium tetrachloride is added into 3.0L ethylene glycol, is heated to flowing back, 0.5L water and four is added
Titanium chloride reaction is cooled to room temperature, is centrifuged, washs, obtain two-dimensional ultrathin nano-TiO after reacting 2.0h2。
By two-dimensional ultrathin nano-TiO2It is counter to be scattered in water and alcohol mixed solution (water and ethyl alcohol volume ratio be 9:1), surpass
Then surfactant KH550 is added in scattered 50min estranged, 4h is reacted at 70 DEG C, and 5000r/min is centrifuged after cooling, and 100 DEG C
Under be dried overnight, the additional amount of the surfactant is two-dimensional ultrathin nano-TiO2The 5% of quality;Obtain modified two dimension
Ultrathin nanometer TiO2- M (with a thickness of 20nm, radius-thickness ratio 15).
By PBT material and modified two-dimensional ultrathin nanometer sheet TiO2- M is dry, and drying temperature is 110 DEG C, drying time 6
Hour, the spinnability of fiber can be improved;Then in parts by weight by PBT material: 96 parts, modified two-dimensional ultrathin nano-TiO2-
M:0.5 parts, antioxidant 1076: 1 part, PETS-XY201A:2.5 parts of lubricant are stirred and mix to uniform, using melt blending
Method makes mixture squeeze out, be granulated by double screw extruder;Extrusion temperature is 230 DEG C, and screw speed 150r/min is obtained
Pellet;
Pellet is extremely dried in 110 DEG C of vacuum drying ovens again;Pellet is subjected to extrusion spinneret again, temperature is 230 DEG C, through cutting
Obtained composite spun fiber is soaked in progress sharpening processing in 30% NaOH solution after cutting, obtains a kind of two-dimensional ultrathin
TiO2The nano combined brush filament of modified PBT.
The performance test data for the compound brush filament that embodiment 1 is prepared is as shown in table 1.
Embodiment 2
Under nitrogen protection, 0.5L titanium tetrachloride is added into 3.0L ethylene glycol, is heated to flowing back, 0.5L water and four is added
Titanium chloride reaction is cooled to room temperature, is centrifuged, washs, obtain two-dimensional ultrathin nano-TiO after reacting 2.0h2。
By two-dimensional ultrathin nano-TiO2It is counter to be scattered in water and alcohol mixed solution (water and ethyl alcohol volume ratio be 9:1), surpass
Then surfactant KH550 is added in scattered 50min estranged, 4h is reacted at 70 DEG C, and 5000r/min is centrifuged after cooling, and 100 DEG C
Under be dried overnight, the additional amount of the surfactant is two-dimensional ultrathin nano-TiO2The 5% of quality;Obtain modified two dimension
Ultrathin nanometer TiO2- M (with a thickness of 20nm, radius-thickness ratio 15).
By PBT material and modified two-dimensional ultrathin nano-TiO2- M is dry, and drying temperature is 110 DEG C, and drying time is 6 small
When, the spinnability of fiber can be improved;Then PBT material in parts by weight: 95.5 parts, modified two-dimensional ultrathin nano-TiO2- M:
1.0 parts, antioxidant 1010: 1 part, lubricant MoS2: 2.5 parts are stirred and mix to uniform, using melt-blending process, make to mix
Object is squeezed out by double screw extruder, is granulated;Extrusion temperature is 230 DEG C, and screw speed 150r/min obtains pellet;
Pellet is extremely dried in 110 DEG C of vacuum drying ovens again;Pellet is subjected to extrusion spinneret again, temperature is 230 DEG C, through cutting
Obtained composite spun fiber is soaked in progress sharpening processing in 30% NaOH solution after cutting, obtains a kind of two-dimensional ultrathin
TiO2The nano combined brush filament of modified PBT.
Fig. 1 and 2 is respectively the surface sweeping electromicroscopic photograph that pure Direct-spinning of PET Fiber is 250 and 1000 times in enlargement ratio.Fig. 3 and 4 is
The two-dimensional ultrathin nano-TiO that the embodiment of the present invention 2 is prepared2The nano combined spinning of modified poly ester is 650 Hes in enlargement ratio
1000 times of surface sweeping electromicroscopic photograph.It compares with pure Direct-spinning of PET Fiber, fiber surface of the invention has obvious concave-convex sense, illustrates its knot
Structure is similar to wool.
The performance test data for the compound brush filament that embodiment 2 is prepared is as shown in table 1.
Embodiment 3
Under nitrogen protection, 1.0L titanium tetrachloride is added into 5.0L ethylene glycol, is heated to flowing back, 0.8L water and four is added
Titanium chloride reaction is cooled to room temperature, is centrifuged, washs, obtain two-dimensional ultrathin nano-TiO after reacting 4.0h2。
By two-dimensional ultrathin nano-TiO2It is counter to be scattered in water and alcohol mixed solution (water and ethyl alcohol volume ratio be 9:1), surpass
Then surfactant KH560 is added in scattered 50min estranged, 4h is reacted at 70 DEG C, and 5000r/min is centrifuged after cooling, and 100 DEG C
Under be dried overnight, the additional amount of the surfactant is two-dimensional ultrathin nano-TiO2The 5% of quality;Obtain modified two dimension
Ultrathin nanometer TiO2- M (with a thickness of 15nm, radius-thickness ratio 20).
By PET material and modified two-dimensional ultrathin nano-TiO2- M is dry, and drying temperature is 110 DEG C, and drying time is 6 small
When, the spinnability of fiber can be improved;Then PET material in parts by weight: 94 parts, modified two-dimensional ultrathin nano-TiO2- M:2.0
Part, antioxidant 1010: 1 part, PETS-XY201A:3 parts of lubricant are stirred and mix to uniform, using melt-blending process, make to mix
Object is closed to squeeze out, be granulated by double screw extruder;Extrusion temperature is 240 DEG C, and screw speed 150r/min obtains pellet;
Pellet is extremely dried in 110 DEG C of vacuum drying ovens again;Pellet is subjected to extrusion spinneret again, temperature is 235 DEG C, through cutting
Obtained composite spun fiber is soaked in progress sharpening processing in 30% NaOH solution after cutting, obtains a kind of two-dimensional ultrathin
TiO2The nano combined brush filament of modified PET.
The performance test data for the compound brush filament that embodiment 3 is prepared is as shown in table 1.
Embodiment 4
Under nitrogen protection, 1.0L titanium tetrachloride is added into 5.0L ethylene glycol, is heated to flowing back, 0.8L water and four is added
Titanium chloride reaction is cooled to room temperature, is centrifuged, washs, obtain two-dimensional ultrathin nano-TiO after reacting 4.0h2。
By two-dimensional ultrathin nano-TiO2It is counter to be scattered in water and alcohol mixed solution (water and ethyl alcohol volume ratio be 9:1), surpass
Then surfactant KH560 is added in scattered 50min estranged, 4h is reacted at 70 DEG C, and 5000r/min is centrifuged after cooling, and 100 DEG C
Under be dried overnight, the additional amount of the surfactant is two-dimensional ultrathin nano-TiO2The 5% of quality;Obtain modified two dimension
Ultrathin nanometer TiO2- M (with a thickness of 15nm, radius-thickness ratio 20).
By PET material and modified two-dimensional ultrathin nano-TiO2- M is dry, and drying temperature is 110 DEG C, and drying time is 6 small
When, the spinnability of fiber can be improved;Then PET material in parts by weight: 92 parts, modified two-dimensional ultrathin nano-TiO2- M:4
Part, antioxidant 1076: 1 part, lubricant MoS2: 3 parts are stirred and mix to uniform, using melt-blending process, keep mixture logical
Double screw extruder is crossed to squeeze out, be granulated;Extrusion temperature is 240 DEG C, and screw speed 150r/min obtains pellet;
Pellet is extremely dried in 110 DEG C of vacuum drying ovens again;Pellet is subjected to spinning again;Pellet is subjected to extrusion spray again
Silk, temperature are 235 DEG C, and the composite spun fiber that will be obtained after clipped is soaked in 30% NaOH solution and carries out at sharpening
Reason, obtains a kind of two-dimensional ultrathin TiO2The nano combined brush filament of modified PET.
The performance test data for the compound brush filament that embodiment 4 is prepared is as shown in table 1.
Table 1
It is provided for the embodiments of the invention technical solution above to be described in detail, specific case used herein
The principle and embodiment of the embodiment of the present invention are expounded, the explanation of above embodiments is only applicable to help to understand this
The principle of inventive embodiments;Meanwhile for the those skilled in the art in a field, according to an embodiment of the present invention, it is being embodied
There will be changes in mode and in application range, in conclusion the content of the present specification should not be construed as to limit of the invention
System.
Claims (10)
1. a kind of compound brush filament of titania modified polyester nano of two-dimensional ultrathin, which is characterized in that in parts by weight, by with
The following group is grouped as:
60-96 parts of polyester, modified two-dimensional ultrathin nano-TiO20.1-20 parts, 0.5-2 parts of antioxidant, 0.5-8 parts of lubricant;
The two-dimensional ultrathin nano-TiO of the modification2It is by two-dimensional ultrathin nano-TiO2It is modified that surfactant progress surface is added
It obtains afterwards;
The two-dimensional ultrathin nano-TiO of the modification2It is less than 50nm for thickness, radius-thickness ratio is greater than 5.
2. a kind of compound brush filament of the titania modified polyester nano of two-dimensional ultrathin according to claim 1, which is characterized in that
The surfactant is one or both of KH550, KH560 or hexamethyldisilazane.
3. a kind of two-dimensional ultrathin TiO according to claim 12The nano combined brush filament of modified poly ester, which is characterized in that described
Polyester be one of PET or PBT.
4. a kind of compound brush filament of the titania modified polyester nano of two-dimensional ultrathin according to claim 1, which is characterized in that
The antioxidant is one or both of antioxidant 1010,1076, B900,3114.
5. a kind of compound brush filament of the titania modified polyester nano of two-dimensional ultrathin according to claim 1, which is characterized in that
The lubricant is MoS2Or one or both of PETS-XY201A.
6. a kind of preparation method of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin described in claim 1, special
Sign is, comprising:
Step 1: preparation two-dimensional ultrathin nano-TiO2
Under nitrogen protection, titanium tetrachloride is added into ethylene glycol, is heated to flowing back, water reaction is then added, it is super to obtain two dimension
Thin nano-TiO2;
Step 2: modified two-dimensional ultrathin nano-TiO2
By the two-dimensional ultrathin nano-TiO of surfactant and step 12Reaction, obtains modified two-dimensional ultrathin nano-TiO2;
Step 3: melt blending
By polyester, the two-dimensional ultrathin nano-TiO of modification2, antioxidant and lubricant be stirred and mix to mixing that is uniform, obtaining
Object is squeezed out by double screw extruder, is granulated, and pellet is obtained;
Step 4: spinning moulding
The pellet of step 3 is subjected to spinning moulding, obtains two-dimensional ultrathin TiO2The nano combined brush filament of modified poly ester.
7. a kind of preparation method of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin described in claim 1, special
Sign is, the volume ratio of ethylene glycol and titanium tetrachloride is (5-100) in the step 1: 1, the volume ratio of titanium tetrachloride and water is
(1-4): 1.
8. a kind of preparation method of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin described in claim 1, special
Sign is that the reaction temperature of the step two is 60~80 DEG C, reaction time 2-6h.
9. a kind of preparation method of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin described in claim 1, special
Sign is that the extrusion temperature of the step 3 is 220-260 DEG C, screw speed 100-150r/min.
10. a kind of preparation method of the compound brush filament of the titania modified polyester nano of two-dimensional ultrathin described in claim 1, special
Sign is that the spinning moulding temperature of the step 4 is 220-260 DEG C.
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CN116553607B (en) * | 2023-03-28 | 2024-04-12 | 南京大学 | Ultra-thin TiO (titanium dioxide) prepared based on condensation reflux method 2 Method for preparing nanosheets and application thereof |
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