CN109957223B - Inorganic nano-silica modified PBT nano-composite spinning material and preparation method thereof - Google Patents
Inorganic nano-silica modified PBT nano-composite spinning material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/016—Additives defined by their aspect ratio
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Abstract
The invention provides an inorganic nano-silica modified PBT nano-composite spinning material and a preparation method thereof, belonging to the technical field of high polymer materials. The composite spinning material comprises the following components in parts by weight: 60-96 parts of PBT, 0.1-10 parts of modified inorganic nano silica, 0.5-2 parts of antioxidant and 0.5-8 parts of lubricant. The invention also provides a preparation method of the inorganic nano-silica modified PBT nano-composite spinning material. According to the invention, inorganic nano silica is subjected to surface modification, and is filled with PBT, so that the inorganic nano silica is uniformly dispersed in a PBT matrix and has good compatibility, the polyester fiber has good spinnability, the surface of the prepared fiber has obvious concave-convex feeling, and the performance and the structure of the prepared fiber are similar to those of wool.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an inorganic nano-silica modified PBT nano-composite spinning material and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) is an important member of the polyester family, and is synthesized by polycondensation of 1, 4-butanediol and terephthalic acid or terephthalate and is manufactured into a translucent thermoplastic crystalline polymer resin through a mixing and banburying process. The PBT main chain is composed of saturated linear molecules, and the repeating unit of the PBT main chain is composed of rigid benzene rings and flexible fatty alcohol. Because the molecular chain contains benzene ring and lipid group, the PBT has higher rigidity and better flexibility. The sample sending structure has the properties of low water absorption rate and acid and alkali resistance, and due to the regular structure, the PBT can be quickly crystallized at low temperature and has excellent forming and processing performances. The structure ensures that the PBT has good corrosion resistance and weather resistance, and can still maintain excellent electrical insulation and mechanical properties under severe environments such as humidity. In addition, the molecules have no side chain and are symmetrical in structure, so that the molecules can be closely packed, and the PBT has the comprehensive properties of higher crystallinity, higher melting point and the like. However, the PBT product has two defects of easy bending and large notch sensitivity, thereby causing certain influence on the industrial application of the PBT. In order to make the PBT have more perfect performance, inorganic filling modified polymer resin is generally adopted, so that the cost is controlled, and the performance of the PBT is improved. The inorganic filler has special physical and chemical properties, and can obviously improve the mechanical property, the forming property, the thermal property and the like of the polymer, so the inorganic filler is rapidly applied and developed in the polymer modification technology.
The surface modification treatment is carried out on the inorganic filler by adding the surfactant, so that the filler is uniformly distributed in a polymer filling system, and an interface with good compatibility is formed between the filler and a polymer polyester matrix, thereby improving the performance of the PBT.
Disclosure of Invention
The invention aims to provide an inorganic nano silica modified PBT nano composite spinning material and a preparation method thereof.
The invention firstly provides an inorganic nano-silica modified PBT nano-composite spinning material which comprises the following components in parts by weight:
60-96 parts of PBT, 0.1-10 parts of modified inorganic nano silica, 0.5-2 parts of antioxidant and 0.5-8 parts of lubricant.
Preferably, the preparation method of the modified inorganic nano silica comprises the following steps:
mixing and grinding flaky aluminum potassium silicate, a dispersing agent, a surfactant and deionized water to obtain modified inorganic nano silica; the thickness of the flaky potassium aluminum silicate is less than or equal to 200nm, and the diameter-thickness ratio is 10-20.
Preferably, the mass percentages of the flaky potassium aluminum silicate, the dispersing agent, the silane coupling agent and the deionized water are 50: 10: 2: 38.
preferably, the grinding time is 6-10 h.
Preferably, the surfactant is one or more of KH550, KH560 and hexamethyldisilazane.
Preferably, the dispersant is BYK-110, FS-5118 or BYK 163.
Preferably, the antioxidant is one or more of antioxidants 1010 or 1076.
Preferably, the lubricant is MoS2Or 3853.
The invention also provides a preparation method of the inorganic nano-silica modified PBT nano-composite spinning material, which comprises the following steps:
stirring and mixing the PBT material, the modified inorganic nano silica, the antioxidant and the lubricant until the mixture is uniform, extruding the mixture by a double-screw extruder by adopting a melt blending method, and granulating and drying; and extruding and spinning the granules to obtain the inorganic nano silica modified PBT nano composite spinning material.
Preferably, the extrusion temperature in the double-screw extruder is 220-260 ℃, and the extrusion spinning temperature in the single-screw extruder is 220-280 ℃.
The invention has the advantages of
The invention provides an inorganic nano-silica modified PBT nano composite spinning material and a preparation method thereof, the material is prepared by adding modified inorganic nano-silica into a PBT material, surface modification is carried out on the inorganic nano-silica, and the inorganic nano-silica is used for filling PBT, so that the inorganic nano-silica is uniformly dispersed in a PBT matrix and has good compatibility, polyester fibers have good spinnability, the surface of prepared fibers has obvious concave-convex feeling, the performance and the structure of the fiber are similar to those of wool, the defects of low powder-sticking rate, poor powder-releasing effect and the like of the conventional artificial brush filaments are overcome, and the requirements of the cosmetic industry on cosmetic brushes are met. The product has high added value, and can be widely applied to toothbrushes, dust removing brushes, various brushes in the cosmetic industry and the like.
Drawings
FIG. 1 is a scanning electron micrograph of pure PBT at a magnification of 500;
FIG. 2 is a scanning electron micrograph of pure PBT at 1000 times;
FIG. 3 is a photograph of a pure PBT by scanning electron microscope with a magnification of 5000;
FIG. 4 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning of example 3 at a magnification of 250;
FIG. 5 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning of example 3 at a magnification of 1200;
FIG. 6 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning prepared in example 3 at a magnification of 3000.
Detailed Description
The invention firstly provides an inorganic nano-silica modified PBT nano-composite spinning material which comprises the following components in parts by weight:
60-96 parts of PBT, 0.1-10 parts of modified inorganic nano silica, 0.5-2 parts of antioxidant and 0.5-8 parts of lubricant; preferably 97.1 to 97.4 parts of PBT, 0.1 to 0.5 part of modified inorganic nano silica, 1 part of antioxidant and 1.5 parts of lubricant;
according to the invention, the preparation method of the modified inorganic nano silica comprises the following steps:
mixing and grinding flaky aluminum potassium silicate, a dispersing agent, a surfactant and deionized water to obtain modified inorganic nano silica; the thickness of the flaky potassium aluminum silicate is less than or equal to 200nm, and the value range of the diameter-thickness ratio is 10-20. When the diameter-thickness ratio is more than 20, the spinnability of the nano composite brush filaments is influenced; when the diameter-thickness ratio is less than 10, the microstructure of the surface of the nano composite brush wire has no obvious change, and the expected powder adhesion effect cannot be achieved. The mass percentage of the flaky potassium aluminum silicate, the dispersing agent, the silane coupling agent and the deionized water is preferably 50: 10: 2: 38.
according to the invention, the grinding is carried out by means commonly used in the art, without any particular limitation, and the grinding time is preferably 6 to 10 hours.
According to the invention, the surfactant is preferably one or more of KH550, KH560 and hexamethyldisilazane; the dispersant is preferably BYK-110, FS-5118 or BYK 163.
According to the invention, the antioxidant is preferably one or more of antioxidant 1010 or antioxidant 1076, and the lubricant is MoS2Or 3853.
The invention also provides a preparation method of the inorganic nano-silica modified PBT nano-composite spinning material, which comprises the following steps:
stirring and mixing the PBT material, the modified inorganic nano-silica, the antioxidant and the lubricant until the mixture is uniform, extruding and granulating the mixture by a double-screw extruder by adopting a melt blending method, and drying the granules in a vacuum oven at the temperature of 100-; and extruding and spinning the granules, cutting, soaking the obtained composite spinning fiber in NaOH solution, and sharpening to obtain inorganic nano silica modified PBT nano composite spinning, thus obtaining the inorganic nano silica modified PBT nano composite spinning material. The extrusion temperature in the double-screw extruder is preferably 220-260 ℃, and the extrusion spinning temperature in the single-screw extruder is preferably 220-280 ℃.
The present invention is described in further detail below with reference to specific examples, in which the starting materials are all commercially available.
Example 1
Removing dust and impurities of flaky potassium aluminum silicate (the diameter-thickness ratio is 10 and the thickness is 200nm), taking 50 parts of flaky potassium aluminum silicate, 16310 parts of dispersing agent BYK, 5602 parts of silane coupling agent KH and 38 parts of deionized water, grinding for 10h by a high-speed wet method, and performing spray drying to obtain modified inorganic nano silica;
the PBT material and the modified inorganic nano silica are dried at the drying temperature of 125 ℃ for 4h, so that the spinnability of the fiber can be improved; the PBT material comprises the following components in parts by weight: 97.4 parts of modified inorganic nano silica: 0.1 part, antioxidant 1010: 1.0 part, lubricant 3853: 1.5 parts of the raw materials are stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 270 deg.c, and stoving in 125 deg.c vacuum oven; extruding and spinning the granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the inorganic nano-silica modified PBT nano-composite spinning is obtained.
Example 2
Removing dust and impurities of flaky potassium aluminum silicate (the diameter-thickness ratio is 10 and the thickness is 200nm), taking 50 parts of flaky potassium aluminum silicate, 16310 parts of dispersing agent BYK, 5602 parts of silane coupling agent KH and 38 parts of deionized water, grinding for 10h by a high-speed wet method, and performing spray drying to obtain modified inorganic nano silica;
the PBT material and the modified inorganic nano silica are dried at the drying temperature of 125 ℃ for 4h, so that the spinnability of the fiber can be improved; the PBT material comprises the following components in parts by weight: 97.3 parts of modified inorganic nano silica: 0.2 part, antioxidant 1010: 1.0 part, lubricant 3853: 1.5 parts of the raw materials are stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 270 deg.c, and stoving in 125 deg.c vacuum oven; extruding and spinning the granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the inorganic nano-silica modified PBT nano-composite spinning is obtained.
Example 3
Removing dust and impurities of flaky potassium aluminum silicate (the diameter-thickness ratio is 10 and the thickness is 200nm), taking 50 parts of flaky potassium aluminum silicate, 16310 parts of dispersing agent BYK, 5602 parts of silane coupling agent KH and 38 parts of deionized water, grinding for 10h by a high-speed wet method, and performing spray drying to obtain modified inorganic nano silica;
the PBT material and the modified inorganic nano silica are dried at the drying temperature of 125 ℃ for 4h, so that the spinnability of the fiber can be improved; the PBT material comprises the following components in parts by weight: 97.2 parts of modified inorganic nano silica: 0.3 part, antioxidant 1076: 1.0 part of lubricant MoS2: 1.5 parts of the raw materials are stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 270 deg.c, and stoving in 125 deg.c vacuum oven; extruding and spinning the granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the inorganic nano-silica modified PBT nano-composite spinning is obtained.
FIG. 4 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning of example 3 at a magnification of 250;
FIG. 5 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning of example 3 at a magnification of 1200;
FIG. 6 is a scanning electron micrograph of the inorganic nano-silica modified PBT nanocomposite spinning prepared according to example 3 at a magnification of 3000;
example 4
Removing dust and impurities of flaky potassium aluminum silicate (the diameter-thickness ratio is 10 and the thickness is 200nm), taking 50 parts of flaky potassium aluminum silicate, 16310 parts of dispersing agent BYK, 5602 parts of silane coupling agent KH and 38 parts of deionized water, grinding for 10h by a high-speed wet method, and performing spray drying to obtain modified inorganic nano silica;
the PBT material and the modified inorganic nano silica are dried at the drying temperature of 125 ℃ for 4h, so that the spinnability of the fiber can be improved; the PBT material comprises the following components in parts by weight: 97 parts of modified inorganic nano silica: 0.5 part, antioxidant 1076: 1.0 part of lubricant MoS2: 1.5 parts of the raw materials are stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 270 deg.c, and stoving in 125 deg.c vacuum oven; extruding and spinning the granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the inorganic nano-silica modified PBT nano-composite spinning is obtained.
Comparative example 1
The PBT material is dried for 4 hours at 125 ℃, so that the spinnability of the fiber can be improved; extruding and spinning pure PBT granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the pure PBT spinning is obtained.
FIGS. 1 to 3 are SEM photographs of pure PBT at 500, 1000 and 5000 magnifications in spinning; from the comparison between fig. 4-6 and fig. 1-3, it can be seen that the composite spinning surface of the nano silica modified PBT has a rough microstructure, and the microstructure can effectively improve the average sticky powder amount of the spinning.
Comparative example 2
Removing dust and impurities of flaky potassium aluminum silicate (the diameter-thickness ratio is 5 and the thickness is 200nm), taking 50 parts of flaky potassium aluminum silicate, 16310 parts of dispersing agent BYK, KH 5602 parts of silane coupling agent and 38 parts of deionized water, grinding for 10 hours by a high-speed wet method, and performing spray drying to obtain modified inorganic nano silica;
the PBT material and the modified inorganic nano silica are dried at the drying temperature of 125 ℃ for 4h, so that the spinnability of the fiber can be improved; the PBT material comprises the following components in parts by weight: 97 parts of modified inorganic nano silica: 0.5 part, antioxidant 1076: 1.0 part of lubricant MoS2: 1.5 parts of the raw materials are stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 270 deg.c, and stoving in 125 deg.c vacuum oven; extruding and spinning the granules; the highest spinning temperature is 275 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the inorganic nano-silica modified PBT nano-composite spinning is obtained.
The viscose powder amount test data of the composite spun yarns obtained in examples 1 to 4 and comparative examples 1 to 2 are shown in table 1:
TABLE 1
As can be seen from Table 1, compared with pure PBT spinning, the composite spinning powder of the invention has better sticky powder effect, and meanwhile, compared with comparative example 2, when the radius-thickness ratio of the flaky potassium aluminum silicate is too h, the microstructure of the surface of the nano composite brush wire has no obvious change and can not achieve the expected sticky powder effect, so the radius-thickness ratio and the thickness of the flaky potassium aluminum silicate are reasonably controlled.
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (9)
1. The inorganic nano-silica modified PBT nano-composite spinning material is characterized by comprising the following components in parts by weight:
60-96 parts of PBT, 0.1-10 parts of modified inorganic nano silica, 0.5-2 parts of antioxidant and 0.5-8 parts of lubricant
The preparation method of the modified inorganic nano silica comprises the following steps:
mixing and grinding flaky aluminum potassium silicate, a dispersing agent, a surfactant and deionized water to obtain modified inorganic nano silica; the thickness of the flaky potassium aluminum silicate is less than or equal to 200nm, and the diameter-thickness ratio is 10-20.
2. The inorganic nano-silica modified PBT nanocomposite spinning material of claim 1, wherein the mass percentages of the flaky potassium aluminum silicate, the dispersant, the silane coupling agent and the deionized water are 50: 10: 2: 38.
3. the inorganic nano-silica modified PBT nanocomposite spun material of claim 1, wherein the grinding time is 6-10 h.
4. The inorganic nano-silica modified PBT nanocomposite spinning material of claim 1, wherein the surfactant is one or more of KH550, KH560 and hexamethyldisilazane.
5. The inorganic nano silica modified PBT nano composite spinning material of claim 1, wherein the dispersant is BYK-110, FS-5118 or BYK 163.
6. The inorganic nano silica modified PBT nanocomposite spinning material of claim 1, wherein the antioxidant is one or more of antioxidant 1010 or antioxidant 1076.
7. The inorganic nano-silica modified PBT nanocomposite spinning material of claim 1, wherein the lubricant is MoS2。
8. The preparation method of the inorganic nano silica modified PBT nano composite spinning material according to the claim 1, which is characterized by comprising the following steps:
stirring and mixing the PBT material, the modified inorganic nano silica, the antioxidant and the lubricant until the mixture is uniform, extruding the mixture by a double-screw extruder by adopting a melt blending method, and granulating and drying; and extruding and spinning the granules to obtain the inorganic nano silica modified PBT nano composite spinning material.
9. The method for preparing the inorganic nano-silica modified PBT nano-composite spinning material as claimed in claim 8, wherein the extrusion temperature in the twin-screw extruder is 220-260 ℃ and the extrusion spinning temperature in the single-screw extruder is 220-280 ℃.
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