CN112538261A - Method for preparing functional master batch with high solid content and good interface compatibility - Google Patents
Method for preparing functional master batch with high solid content and good interface compatibility Download PDFInfo
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- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- 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
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- 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
- D01F6/90—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 polyamides
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- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a method for preparing functional master batches with high solid content and good interface compatibility, which comprises the steps of carrying out powder refining treatment, drying polyamide slices, carrying out surface treatment on titanium dioxide powder, carrying out modification treatment on polyester powder, mixing with etherimide powder, mixing perovskite composite oxide powder, absolute ethyl alcohol and a dispersing agent to obtain static supplementary emulsion, preparing antibacterial powder from bamboo fibers, carrying out co-stirring on the powder and the static supplementary emulsion to obtain functional powder, carrying out melt blending and extrusion on the functional powder and the polyamide slices, cooling and pelletizing to prepare the functional master batches; the functional master batch prepared by the method has flame retardant, ultraviolet resistant and antibacterial capabilities, has static electricity supplementing capability and can effectively block bacteria, and the functional master batch prepared by the method has high solid content, and can ensure good interface compatibility among materials in the prepared functional master batch by thinning treatment, surface treatment, modification treatment and control of the particle size of powder.
Description
Technical Field
The invention relates to the technical field of preparation and processing of high polymer materials, in particular to a method for preparing functional master batches with high solid content and good interface compatibility.
Background
The nylon fiber is the first synthetic fiber in the world, has the characteristics of high strength, good wear resistance, light weight, small fabric density and the like, and is suitable for being used as mountaineering wear, winter clothes and the like. As a large category of synthetic fibers, the annual yield of chinlon in China is maintained to be more than 300 million tons since 2017. With the improvement of living standard and the requirement of healthy life, some functional fibers come out.
The functional master batch for preparing the functional fiber is mainly characterized in that the resin performance is changed by adding a functional material into a basic resin material to realize the functionality, but the functional material and the basic resin material are not easy to be uniformly dispersed by a physical method, the interfacial compatibility, the dispersibility and the affinity among the materials are poor, and meanwhile, the solid content of the functional material in the prepared functional master batch is low, so that the mechanical property of the material is further reduced. Therefore, the invention provides a method for preparing the functional master batch with high solid content and good interface compatibility, and aims to overcome the defects in the prior art.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for preparing a functional master batch with high solid content and good interface compatibility, the functional master batch prepared by the method has flame retardant, ultraviolet resistant and antibacterial capabilities, and has electrostatic replenishment capability, when the functional master batch is prepared into a functional fiber applied to textile products, bacteria can be effectively blocked by utilizing the electrostatic replenishment capability, and the functional master batch prepared by the method has high solid content, and the interface compatibility among materials in the prepared functional master batch can be ensured by performing refining treatment, surface treatment, modification treatment and controlling the particle size of powder.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme:
the method for preparing the functional master batch with high solid content and good interface compatibility comprises the following steps:
the method comprises the following steps: preparing polyamide slices, titanium dioxide powder, polyetherimide powder, polyester powder, chitin powder, graphene powder, bamboo fiber and perovskite composite oxide powder, and then respectively refining the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder and the graphene powder;
step two: drying polyamide slices until the water content is less than 35ppm, and then performing surface treatment on titanium dioxide powder by using a surface treatment agent A, wherein the amount of the surface treatment agent is 0.2-0.6% of the mass of the titanium dioxide powder;
step three: modifying polyester powder by using a modifier, and then mixing the modified polyester powder with ether imide powder to obtain a mixture for later use;
step four: mixing the perovskite composite oxide powder with absolute ethyl alcohol and a dispersing agent, and stirring by using a high-speed shearing machine after mixing to obtain static electricity supplementing emulsion;
step five: soaking the bamboo fiber in a surface treating agent B, and then drying and grinding to prepare antibacterial powder;
step six: mixing the titanium dioxide powder subjected to surface treatment, the mixture, the chitin powder, the graphene powder, the antibacterial powder and the static supplementary emulsion together, and drying to obtain functional powder;
step seven: functional powder and polyamide chips are mixed according to the mass ratio of 1: 1.5-4, and finally cooling and granulating to prepare the functional master batch.
The further improvement lies in that: in the first step, the titanium dioxide powder is rutile titanium dioxide powder, the particle size of the refined titanium dioxide powder is controlled to be 0.2-0.3 mu m, the particle size of the refined polyetherimide powder and the refined polyester powder is controlled to be 20-60 mu m, and the particle size of the refined chitin powder and the refined graphene powder is controlled to be 10-50 mu m.
The further improvement lies in that: and in the second step, the surface treating agent A is a titanate coupling agent or a silane coupling agent, and when the surface treating agent A is the silane coupling agent, the surface treating agent A is specifically any one of gamma-aminopropyltriethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane.
The further improvement lies in that: the process of carrying out surface treatment on the titanium dioxide powder by using the surface treating agent A in the step two is as follows: mixing titanium dioxide and an organic ultraviolet absorbent in a ratio of 1: 10-30, adding a coupling agent, adding water to fully perform hydrolysis reaction to generate a composite anti-ultraviolet material, and drying and grinding the composite anti-ultraviolet material to obtain composite anti-ultraviolet powder with uniform particle size.
The further improvement lies in that: and in the third step, the modifier is a flame retardant, and the flame retardant is polybrominated diphenyl ether, in particular decabrominated diphenyl ether.
The further improvement lies in that: and in the step five, the surface treating agent B is formed by mixing a silane coupling agent and anhydrous methanol according to the mass ratio of 1: 10.
The further improvement lies in that: and in the sixth step, the drying temperature is 120-180 ℃, and the water content of the dried functional powder is less than 50 ppm.
The further improvement lies in that: and seventhly, before the functional powder and the polyamide slices are mixed, the polyamide slices need to be crushed, and the polyamide slices are crushed to 20-30 meshes by adopting a freezing and crushing mode in the crushing treatment, so that the polyamide powder is obtained.
The further improvement lies in that: and seventhly, controlling the stirring speed to be 160-200 r/min when the neutral powder and the polyamide powder are subjected to melt blending, wherein the stirring process is carried out in a nitrogen atmosphere, and the melt blending temperature is 240-270 ℃.
The invention has the beneficial effects that: the functional master batch prepared from the polyamide chips, the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder, the graphene powder, the bamboo fiber and the perovskite composite oxide powder has flame retardant, ultraviolet resistant and antibacterial capabilities and electrostatic supplementation capability, and the functional fiber prepared from the functional master batch can effectively block bacteria by utilizing the electrostatic supplementation capability when applied to textile products.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example one
As shown in fig. 1, the embodiment provides a method for preparing a functional masterbatch with high solid content and good interface compatibility, which includes the following steps:
the method comprises the following steps: preparing polyamide chips, titanium dioxide powder, polyetherimide powder, polyester powder, chitin powder, graphene powder, bamboo fiber and perovskite composite oxide powder, and then respectively refining the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder and the graphene powder, wherein the titanium dioxide powder is rutile titanium dioxide powder, the grain size of the refined titanium dioxide powder is controlled to be 0.2 mu m, the grain size of the refined polyetherimide powder and the refined polyester powder is controlled to be 20 mu m, and the grain size of the refined chitin powder and the refined graphene powder is controlled to be 10 mu m;
step two: drying polyamide slices until the water content of the polyamide slices is less than 35ppm, and then performing surface treatment on titanium dioxide powder by using a surface treatment agent A, wherein the using amount of the surface treatment agent is 0.4% of the mass of the titanium dioxide powder, the surface treatment agent A is a silane coupling agent, specifically gamma-aminopropyltriethoxysilane, and the surface treatment process comprises the following steps: mixing titanium dioxide and an organic ultraviolet absorbent in a ratio of 1:10 in the ethanol solution, adding a coupling agent, adding water to fully perform hydrolysis reaction to generate a composite anti-ultraviolet material, and drying and grinding the composite anti-ultraviolet material to obtain composite anti-ultraviolet powder with uniform particle size;
step three: modifying polyester powder by using a modifier, and then mixing the modified polyester powder with ether imide powder to obtain a mixture for later use, wherein the modifier is a flame retardant, and specifically is decabromodiphenyl ether;
step four: mixing the perovskite composite oxide powder with absolute ethyl alcohol and a dispersing agent, and stirring by using a high-speed shearing machine after mixing to obtain static electricity supplementing emulsion;
step five: soaking bamboo fibers with a surface treatment agent B, drying and grinding to prepare antibacterial powder, wherein the surface treatment agent B is formed by mixing a silane coupling agent and anhydrous methanol according to a mass ratio of 1: 10;
step six: mixing the titanium dioxide powder subjected to surface treatment, the mixture, the chitin powder, the graphene powder, the antibacterial powder and the static supplementary emulsion together, and drying to obtain functional powder, wherein the drying temperature is 160 ℃, and the water content of the dried functional powder is less than 50 ppm;
step seven: and (2) crushing the polyamide chips into 25 meshes by adopting a freezing and crushing mode to obtain polyamide powder, wherein the functional powder and the polyamide powder are mixed according to a mass ratio of 1: 1.5, performing melt blending and extrusion, finally performing cooling and grain cutting to prepare functional master batches, controlling the stirring speed to be 180r/min during blending, performing the stirring process in a nitrogen atmosphere, and performing melt blending at the temperature of 260 ℃.
Example two
As shown in fig. 1, the embodiment provides a method for preparing a functional masterbatch with high solid content and good interface compatibility, which includes the following steps:
the method comprises the following steps: preparing polyamide chips, titanium dioxide powder, polyetherimide powder, polyester powder, chitin powder, graphene powder, bamboo fiber and perovskite composite oxide powder, and then respectively refining the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder and the graphene powder, wherein the titanium dioxide powder is rutile titanium dioxide powder, the grain size of the refined titanium dioxide powder is controlled to be 0.25 mu m, the grain size of the refined polyetherimide powder and the refined polyester powder is controlled to be 40 mu m, and the grain size of the refined chitin powder and the refined graphene powder is controlled to be 30 mu m;
step two: drying polyamide slices until the water content of the polyamide slices is less than 35ppm, and then performing surface treatment on titanium dioxide powder by using a surface treatment agent A, wherein the using amount of the surface treatment agent is 0.4% of the mass of the titanium dioxide powder, the surface treatment agent A is a silane coupling agent, specifically gamma-aminopropyltriethoxysilane, and the surface treatment process comprises the following steps: mixing titanium dioxide and an organic ultraviolet absorbent in a ratio of 1: 20 in the ethanol solution, adding a coupling agent, adding water to fully perform hydrolysis reaction to generate a composite anti-ultraviolet material, and drying and grinding the composite anti-ultraviolet material to obtain composite anti-ultraviolet powder with uniform particle size;
step three: modifying polyester powder by using a modifier, and then mixing the modified polyester powder with ether imide powder to obtain a mixture for later use, wherein the modifier is a flame retardant, and specifically is decabromodiphenyl ether;
step four: mixing the perovskite composite oxide powder with absolute ethyl alcohol and a dispersing agent, and stirring by using a high-speed shearing machine after mixing to obtain static electricity supplementing emulsion;
step five: soaking bamboo fibers with a surface treatment agent B, drying and grinding to prepare antibacterial powder, wherein the surface treatment agent B is formed by mixing a silane coupling agent and anhydrous methanol according to a mass ratio of 1: 10;
step six: mixing the titanium dioxide powder subjected to surface treatment, the mixture, the chitin powder, the graphene powder, the antibacterial powder and the static supplementary emulsion together, and drying to obtain functional powder, wherein the drying temperature is 160 ℃, and the water content of the dried functional powder is less than 50 ppm;
step seven: and (2) crushing the polyamide chips into 25 meshes by adopting a freezing and crushing mode to obtain polyamide powder, wherein the functional powder and the polyamide powder are mixed according to a mass ratio of 1: 3, performing melt blending and extrusion, finally performing cooling and grain cutting to prepare functional master batches, controlling the stirring speed to be 180r/min during blending, performing the stirring process in a nitrogen atmosphere, and performing melt blending at the temperature of 260 ℃.
EXAMPLE III
As shown in fig. 1, the embodiment provides a method for preparing a functional masterbatch with high solid content and good interface compatibility, which includes the following steps:
the method comprises the following steps: preparing polyamide chips, titanium dioxide powder, polyetherimide powder, polyester powder, chitin powder, graphene powder, bamboo fiber and perovskite composite oxide powder, and then respectively refining the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder and the graphene powder, wherein the titanium dioxide powder is rutile titanium dioxide powder, the grain size of the refined titanium dioxide powder is controlled to be 0.3 mu m, the grain size of the refined polyetherimide powder and the refined polyester powder is controlled to be 60 mu m, and the grain size of the refined chitin powder and the refined graphene powder is controlled to be 50 mu m;
step two: drying polyamide slices until the water content of the polyamide slices is less than 35ppm, and then performing surface treatment on titanium dioxide powder by using a surface treatment agent A, wherein the using amount of the surface treatment agent is 0.4% of the mass of the titanium dioxide powder, the surface treatment agent A is a silane coupling agent, specifically gamma-aminopropyltriethoxysilane, and the surface treatment process comprises the following steps: mixing titanium dioxide and an organic ultraviolet absorbent in a ratio of 1: 30 in proportion, adding a coupling agent, adding water to fully perform hydrolysis reaction to generate a composite anti-ultraviolet material, and drying and grinding the composite anti-ultraviolet material to obtain composite anti-ultraviolet powder with uniform particle size;
step three: modifying polyester powder by using a modifier, and then mixing the modified polyester powder with ether imide powder to obtain a mixture for later use, wherein the modifier is a flame retardant, and specifically is decabromodiphenyl ether;
step four: mixing the perovskite composite oxide powder with absolute ethyl alcohol and a dispersing agent, and stirring by using a high-speed shearing machine after mixing to obtain static electricity supplementing emulsion;
step five: soaking bamboo fibers with a surface treatment agent B, drying and grinding to prepare antibacterial powder, wherein the surface treatment agent B is formed by mixing a silane coupling agent and anhydrous methanol according to a mass ratio of 1: 10;
step six: mixing the titanium dioxide powder subjected to surface treatment, the mixture, the chitin powder, the graphene powder, the antibacterial powder and the static supplementary emulsion together, and drying to obtain functional powder, wherein the drying temperature is 160 ℃, and the water content of the dried functional powder is less than 50 ppm;
step seven: and (2) crushing the polyamide chips into 25 meshes by adopting a freezing and crushing mode to obtain polyamide powder, wherein the functional powder and the polyamide powder are mixed according to a mass ratio of 1: 4, performing melt blending and extrusion, finally performing cooling and grain cutting to prepare functional master batches, controlling the stirring speed to be 180r/min during blending, performing the stirring process in a nitrogen atmosphere, and performing melt blending at the temperature of 260 ℃.
The invention relates to a method for blocking bacteria and viruses on textiles, which is characterized in that the bacteria and the viruses are adsorbed on the textiles through static electricity, and then the bacteria and the viruses are prevented from passing through the textiles to be contacted with human skin, but the textiles can cause static electricity loss in the wearing, cleaning and contacting processes with water in the air, so that the antibacterial ability is reduced, perovskite composite oxides are used as raw materials for preparing master batches, and the perovskite composite oxides have stable crystal structures, unique electromagnetic properties and high activities such as oxidation reduction, hydrogenolysis, isomerization, electrocatalysis and the like, when the prepared functional master batches are used for the textiles, the dipoles of the perovskite composite oxides are not superposed when the temperature is changed, so that current is induced to be generated, the charges are accumulated according to the direction of dipole points, and certain areas can attract or repel the charges when the textile materials are deformed, then current is generated again to complete the static electricity supplement of the fabric, thereby improving the capability of blocking bacteria and viruses.
The functional master batch prepared from the polyamide chips, the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder, the graphene powder, the bamboo fiber and the perovskite composite oxide powder has flame retardant, ultraviolet resistant and antibacterial capabilities and electrostatic supplementation capability, and the functional fiber prepared from the functional master batch can effectively block bacteria by utilizing the electrostatic supplementation capability when applied to textile products.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The method for preparing the functional master batch with high solid content and good interface compatibility is characterized by comprising the following steps:
the method comprises the following steps: preparing polyamide slices, titanium dioxide powder, polyetherimide powder, polyester powder, chitin powder, graphene powder, bamboo fiber and perovskite composite oxide powder, and then respectively refining the titanium dioxide powder, the polyetherimide powder, the polyester powder, the chitin powder and the graphene powder;
step two: drying polyamide slices until the water content is less than 35ppm, and then performing surface treatment on titanium dioxide powder by using a surface treatment agent A, wherein the amount of the surface treatment agent is 0.2-0.6% of the mass of the titanium dioxide powder;
step three: modifying polyester powder by using a modifier, and then mixing the modified polyester powder with ether imide powder to obtain a mixture for later use;
step four: mixing the perovskite composite oxide powder with absolute ethyl alcohol and a dispersing agent, and stirring by using a high-speed shearing machine after mixing to obtain static electricity supplementing emulsion;
step five: soaking the bamboo fiber in a surface treating agent B, and then drying and grinding to prepare antibacterial powder;
step six: mixing the titanium dioxide powder subjected to surface treatment, the mixture, the chitin powder, the graphene powder, the antibacterial powder and the static supplementary emulsion together, and drying to obtain functional powder;
step seven: functional powder and polyamide chips are mixed according to the mass ratio of 1: 1.5-4, and finally cooling and granulating to prepare the functional master batch.
2. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: in the first step, the titanium dioxide powder is rutile titanium dioxide powder, the particle size of the refined titanium dioxide powder is controlled to be 0.2-0.3 mu m, the particle size of the refined polyetherimide powder and the refined polyester powder is controlled to be 20-60 mu m, and the particle size of the refined chitin powder and the refined graphene powder is controlled to be 10-50 mu m.
3. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: and in the second step, the surface treating agent A is a titanate coupling agent or a silane coupling agent, and when the surface treating agent A is the silane coupling agent, the surface treating agent A is specifically any one of gamma-aminopropyltriethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane.
4. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: the process of carrying out surface treatment on the titanium dioxide powder by using the surface treating agent A in the step two is as follows: mixing titanium dioxide and an organic ultraviolet absorbent in a ratio of 1: 10-30, adding a coupling agent, adding water to fully perform hydrolysis reaction to generate a composite anti-ultraviolet material, and drying and grinding the composite anti-ultraviolet material to obtain composite anti-ultraviolet powder with uniform particle size.
5. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: and in the third step, the modifier is a flame retardant, and the flame retardant is polybrominated diphenyl ether, in particular decabrominated diphenyl ether.
6. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: and in the step five, the surface treating agent B is formed by mixing a silane coupling agent and anhydrous methanol according to the mass ratio of 1: 10.
7. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: and in the sixth step, the drying temperature is 120-180 ℃, and the water content of the dried functional powder is less than 50 ppm.
8. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 1, which is characterized in that: and seventhly, before the functional powder and the polyamide slices are mixed, the polyamide slices need to be crushed, and the polyamide slices are crushed to 20-30 meshes by adopting a freezing and crushing mode in the crushing treatment, so that the polyamide powder is obtained.
9. The method for preparing the functional master batch with high solid content and good interface compatibility according to claim 8, which is characterized in that: and seventhly, controlling the stirring speed to be 160-200 r/min when the neutral powder and the polyamide powder are subjected to melt blending, wherein the stirring process is carried out in a nitrogen atmosphere, and the melt blending temperature is 240-270 ℃.
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